FY 1997 Budget Summary for DOE Materials Activities

DOE/ER-0734 Energy Materials Coordinating Committee (EMaCC)

Fiscal Year 1997

July 31, 1998

Annual Technical Report

U.S. Department of Energy Office of Energy Research Office of Basic Energy Sciences Division of Materials Sciences This report has been reproduced directly from the best available copy.

Available to DOE and DOE Contractors from the Office of Scientific and Technical Information, P.O. Box 62, Oak Ridge, TN 37831; prices available from (423) 576-8401.

Available to the public from the U.S. Department of Commerce, Technology Administration, National Technical Information Service, Springfield, VA 22161, (703) 487-4650.

® Printed with soy ink on recycled paper DOE/ER-0734 Energy Materials Coordinating Committee (EMaCC)

Fiscal Year 1997 July 31, 1998

Annual Technical Report

U.S. Department of Energy Office of Energy Research Office of Basic Energy Sciences Division of Materials Sciences Germantown, MD 20874-1290 Table of Contents

TABLE OF CONTENTS

Page

Introduction ...... 1 Membership List ...... ;...... 3 Organization of the Report ...... 6 FY 1997 Budget Summary for DOE Materials Activities ...... 7 Distribution of Funds by Office ...... 9

PROGRAM DESCRIPTIONS

OFFICE OF ENERGY EFFICIENCY AND RENEWABLE ENERGY ...... 10 Office of Building Technology, State and Community Programs ...... 12 Office of Building Systems ...... 13

OFFICE OF INDUSTRIAL TECHNOLOGIES ...... 15 Office of Industrial Strategies ...... 19 Aluminum Vision Team ...... 19 Forest Products Vision Team ...... 22 Steel Vision Team ...... 23 Glass Vision Team ...... 23 Metal Casting Vision Team ...... 24 Office of Crosscut Technologies ...... 27 Advanced Turbine System (ATS) Program ...... 28 Continuous Fiber Ceramic Composites (CFCC) Program ...... 28 Advanced Industrial Materials (AIM) Program ...... 29 Combustion/Heat Exchanger Program ...... 34

OFFICE OF TRANSPORTATION TECHNOLOGIES ...... 35 Transportation Materials Technology ...... 39 Automotive Materials Technology ...... 39 Propulsion Systems Materials ...... 39 Lightweight Vehicle Materials Technology ...... 42 Electric Drive Vehicle Technology ...... 45 Advanced Battery Program ...... 45 Fuel Cell Materials ...... 50 Heavy Vehicle Materials Technology ...... 50

i Table of Contents

TABLE OF CONTENTS (continued)

Pape OFFICE OF ENERGY EFFICIENCY AND RENEWABLE ENERGY (continued) Office of Utility Technologies ...... 57 Office of Solar Energy Conversion ...... 58 Photovoltaic Energy Technology Division ...... 58 Office of Geothermal Technologies ...... 59 Office of Energy Management ...... 62 Advanced Utility Concepts Division ...... 62 High Temperature Superconductivity for Electric Systems ...... 62

OFFICE OF ENERGY RESEARCH ...... 66 Office of Basic Energy Sciences ...... 79 Division of Materials Sciences ...... 79 Division of Chemical Sciences ...... 81 Division of Engineering and Geosciences ...... 82 Engineering Sciences Research ...... 82 Geosciences Research ...... 92 Office of Computational and Technology Research ...... 99 Division of Advanced Energy Projects and Technology Research ...... 99 Laboratory Technology Research (LTR) Program ...... 99 Advanced Energy Projects Program ...... 118 Small Business Innovation Research Program ...... 127 Small Business Technology Transfer Program ...... 135 Office of Fusion Energy Sciences ...... 135

OFFICE OF ENVIRONMENTAL MANAGEMENT ...... 140

OFFICE OF NUCLEAR ENERGY, SCIENCE AND TECHNOLOGY ...... 150 Office of Engineering and Technology Development ...... 151 Space and National Security Programs ...... 151 Office of Naval Reactors ...... 152

OFFICE OF CIVILIAN RADIOACTIVE WASTE MANAGEMENT ...... 153

OFFICE OF DEFENSE PROGRAMS ...... 155 The Weapons Research, Development and Test Program ...... 158 Sandia National Laboratories ...... 158 Lawrence Livermore National Laboratory ...... 167 Los Alamos National Laboratory ...... 172

Ii Table of Contents

TABLE OF CONTENTS (continued)

OFFICE OF FOSSIL ENERGY ...... 176 Office of Advanced Research ...... 178 Fossil Energy AR&TD Materials Program ...... 178

DIRECTORY ...... 191

IND EX ...... 22 1

iii Introduction

INTRODUCTION

The DOE Energy Materials Coordinating Committee (EMaCC) serves primarily to enhance coordination among the Department's materials programs and to further effective use of materials expertise within the Department. These functions are accomplished through the exchange of budgetary and planning information among program managers and through technical meetings/workshops on selected topics involving both DOE and major contractors. In addition, EMaCC assists in obtaining materials-related inputs for both intra- and interagency compilations.

Six topical subcommittees have been established to focus on materials areas of particular importance to the Department; the subcommittees and their respective chairpersons are:

Electrochemical Technologies - Richard Kelly, ER-132, (301) 903-6051 Metals - Sara Dillich, EE-22, (202) 586-7925 Radioactive Waste Containers - Helen Farrell, ER-131, (301) 903-5998 Semiconductors - Jerry Smith, ER-132, (301) 903-4269 Structural Ceramics - Charles Sorrell, EE-232, (202) 586-1514 Superconductivity - James Daley, EE-142, (202) 586-1165

Membership in the EMaCC is open to any Department organizational unit; participants are appointed by Division or Office Directors. The current active membership is listed on pages 3-5.

Six meetings were scheduled for 1998. The dates, themes and speakers are as follows:

November 13, 1997 Subcommittee on Environmental Management Speaker: Helen Farrell

The minutes of the September 9, 1997, EMaCC meeting were accepted. Organizational details regarding EMaCC subcommittees were discussed. Helen Farrell made a presentation on the FY 1998 Environmental Management Science Program (EMSP) Solicitation. The announcement of the solicitation was said to be imminent and that there might be as much as $20 million for new awards in FY98. A draft report from the R&D Council subcommitteeon Technical Coordinating Committees (TCC) was also discussed.

January 15, 1998 Subcommittee on Electrochemical Technologies Speaker: Professor Philip N. Ross, Lawrence Berkeley National Laboratory

JoAnn Milliken welcomed the speaker and members; Richard Kelley introduced the guest speaker, Professor Philip N. Ross, who spoke on Surface Electrochemistry-Past, Present and Future. Dr. Ross traced the history of studies of the electrochemical interface through the development of electron-based spectroscopic analysis to the current in-situ photon-in photon-out methods such as Surface X-ray Scattering (SXS) and Surface-Enhanced Raman Spectroscopy (SERS). Progress in understanding a number of electrode processes such as potential-dependent reconstruction of Au(hkl) surfaces were discussed as was progress towards a carbon monoxide tolerant electrode for fuel cell. JoAnn Milliken described recent advances in the Automotive Fuel Cell Program. Significant accomplishments include the development of a highly efficient direct-hydrogen fuel cell stack system by International Fuel Cells, Inc., and the demonstration of technical feasibility of gasoline-powered PEM fuel cells. The latter achievement is important for the development of fuel cell systems powered by hydrogen generated by on-board fuel processing of gasoline. Utilizing the existing fuel infrastructure will enable early introduction of automotive fuel cells since a hydrogen fueling infrastructure is currently unavailable. Neil Rossmeissl spoke on materials issues in hydrogen research. The emphasis was on hydrogen storage and also hydrogen

1 Introduction

production, which is a high temperature (800-1200°C) process. The minutes of the November 13, 1997, EMaCC meeting were accepted.

March 12,1998 Subcommittee on Metals Speakers: Dr. Michael Kassner, Oregon State University Dr. Phil Mazlasz, Oak Ridge National Laboratory

Sara Dillich welcomed the speakers on behalf of the Metals Subcommittee and gave a brief overview of planned solicitations/activities of the Office of Industrial Technologies. Dr. Michael Kassner spoke on the Metal Forming Project of the DOE Center for Excellence for the Synthesis and Processing of Advanced Materials. The object of the Metal Forming Project (one of eight Center projects) is to develop a scientific understanding of the phenomena relating to forming of aluminum alloys for industrial (especially automotive) applications. Dr. Phil Maziasz spoke on Achieving Perfect Microstructures for dramatically improving creep-strength of stainless steels. This summarized the results of a Cooperative Research and Development Agreement (CRADA) between ORNL utilizing its alloy R&D and process optimization expertise and Solar Turbines, Inc., as the end-user, and Allegheny-Teledyne as the materials (foil) producer. Dr. Kassner and the Metal Forming project are supported by OER/BES/DMS. Dr. Maziasz's research is supported by the FE/ARTD program.

May 21, 1998 Subcommittee on Superconductivity Speakers: Russell Eaton, DOE Golden Field Office Maribel Soto, Office of Naval Research Superconductivity Programs X-D Xiang, Lawrence Berkeley National Laboratory Bill McCallum, Ames Laboratory

JoAnn Milliken called the meeting to order and Chris Platt welcomed our speakers and guests which included Don Gubser from the Naval Research Laboratories. Russell Eaton spoke on the status of the Superconductivity Partnership Initiative which is sponsored by the Superconductivity for Electric Systems Program, Maribel Soto presented a summary of work supported in the Office of Naval Research Superconductivity Programs, X-D Xiang presented work on the Combinatorial Approach to Study of Superconductors and Other Related Oxide Electronic Materials and Bil McCallum described progress toward understanding the Light Rare-Earth Barium Copper Oxide Superconductors.

July 16, 1998 Subcommittee on Semiconductors/Photovoltaics

September 10, 1998 Subcommittee on Environmental Management

The EMaCC reports to the Director of the Office of Energy Research in his or her capacity as overseer of the technical programs of the Department. This annual technical report is mandated by the EMaCC terms of reference. This report summarizes EMaCC activities for FY 1997 and describes the materials research programs of various offices and divisions within the Department.

The Chairman of EMaCC for FY 1997 was Dr. Yok Chen. The compilation of this report was performed by Dr. Tim Fitzsimmons, EMaCC Executive Secretary for FY 1998, with the assistance of FM Technologies, Inc.

Dr. JoAnn Milliken Office of Transportation Technologies EmaCC Chair, FY 1998

2 Membership List

MEMBERSHIP LIST DEPARTMENT OF ENERGY ENERGY MATERIALS COORDINATING COMMITTEE

H I | '|||j||g|||||i||||||^^^^^^N^^^^^ | g g p .,E

Building Technology. State and Community Programs

Building Systems Arun Vohra, EE-41 202/586-2193

Industrial Technologies

Industrial Process Systems Sara Dillich, EE-22 202/586-7925 Toni Marechaux, EE-22 202/586-8501 Brian Volintine, EE-22 202/586-1739 Industrial Crosscut Technologies Charlie Sorrell, EE-23 202/586-1514 Debbie Haught, EE-23 202/586-2211 Pat Hoffman, EE-23 202/586-6074

Transportation Technologies

Automotive Propulsion System Materials Thomas Sebestyen, EE-32 202/586-9727 Automotive Lightweight Vehicle Materials Joseph Carpenter, EE-32 202/586-1022 Advanced Battery Systems Ray Sutula, EE-32 202/586-8064 Fuel Cell Systems JoAnn Milliken, EE-32 202/586-2480 Heavy Vehicle Propulsion System Materials Sidney Diamond, EE-34 202/586-8032 High Strength Weight Reduction Materials Sidney Diamond, EE-34 202/586-8032 High Temperature Materials Laboratory Sidney Diamond, EE-34 202/586-8032

Utility Technologies Wind/Hydro/Ocean Technologies William Richards, EE-121 202/586-5410 Geothermal Technology Raymond LaSala, EE-122 202/586-4198 Photovoltaic Technology Richard King, EE-131 202/586-1693 Advanced Utility Concepts James Daley, EE-142 202/586-1165 Christine Platt, EE-142 202/586-8943 Chris Kang, EE-142 202/586-4563

3 Membership List

Basic Energy Sciences

Materials Sciences Pat Dehmer, ER-10 301/903-3081 Iran L Thomas, ER-13 301/903-3427 Metal and Ceramic Sciences Robert J. Gottschall, ER-131 301/903-3428 Alan Dragoo, ER-131 301/903-3428 Yok Chen, ER-131 301/903-3428 Helen Kerch, ER-131 301/903-3428 Tim Fitzsimmons, ER-131 301/903-9830 Helen Farrell, ER-131 301/903-5998 Solid State Physics and Materials W. Oosterhuis, ER-132 301/903-3426 Chemistry Jerry Smith, ER-132 301/903-3426 Richard Kelly, ER-132 301/903-3426 Manfred Leiser, ER-132 301/903-3426 Chemical Sciences Robert S. Marianelli, ER-14 301/903-5808 Engineering and Geosciences Paula Davidson, ER-15 301/903-5822 Nick Woodward, ER-15 301/903-5822

Technology Research Ted Vojnovich, ER-32 301/903-7484 David Koegel, ER-32 301/903-3159

LaboratoryOperations and Environment. Safety and Health

Environment, Safety and Health Albert Evans, ER-83 301/903-3427 Michael Teresinski, ER-83 301/903-5155

Fusion Energy

Fusion Technologies F. W. (Bill) Wiffen, ER-52 301/903-4963

Waste Operations

Waste Management Projects Doug Tonkay, EM-34 301/903-7212

Science and Technology

Research and Development Chet Miller, EM-34 , 202/586-3952

4 Membership List

Disposition Technologies William Van Dyke, NE-40 301/903-4201 Beverly Cook, NE-40 301/903-4021

Space and Defense Power Systems William Barnett, NE-50 301/903-3097 John Dowicki, NE-50 301/903-7729

Naval Reactors David I. Curtis, NE-60 703/603-5561 Tom Kennedy, NE-60 703/603-1754

Reactor Programs John Warren, NE-80 301/903-491 Bob Lange, NE-80 301/903-2915

Analysis and Verification Alan Berusch, RW-37 202/586-9362

Research and Advanced Technology

Research and Technology Development Bharat Agrawal, DP-16 301/903-2057

Inertial Confinement Fusion Carl B. Hilland, DP-18 301/903-3687

Advanced Research Fred M. Glaser 301/903-2786

5 Organization of the Report

ORGANIZATION OF THE REPORT

The FY 1997 budget summary for DOE Materials Activities is presented on page 7. The distribution of these funds between DOE laboratories, private industry, academia and other organizations is presented in tabular form on page 9.

Following the budget summary is a set of detailed program descriptions for the FY 1997 DOE Materials activities. These descriptions are presented according to the organizational structure of the Department. A mission statement, a budget summary listing the project titles and FY 1997 funding, and detailed project summaries are presented for each Assistant Secretary office and the Office of Energy Research. The project summaries also provide DOE, laboratory, academic and industrial contacts for each project, as appropriate.

6 FY 1997 Budget Summary for DOE Materials Activities

FY 1997 BUDGET SUMMARY FOR DOE MATERIALS ACTIVITIES

(These numbers represent materials-related activities only. They do not include those portions of program budgets which are not materials related.) FY 1997

OFFICE OF BUILDING TECHNOLOGY, STATE AND COMMUNITY PROGRAMS $1,090,000 Office of Building Systems 1,090,000

OFFICE OF INDUSTRIAL TECHNOLOGIES $32,597,505 Office of Industrial Strategies 10,398,309 Aluminum Vision Team 5,071,000 Forest Products Vision Team 1,084,012 Steel Vision Team 455,000 Glass Vision Team 1,228,000 Metal Casting Vision Team 2,560,297 Office of Crosscut Technologies 22,199,196 Advanced Turbine System (ATS) Program - 7,350,000 Continuous Fiber Ceramic Composites (CFCC) Program 8,400,000 Advanced Industrial Materials (AIM) Program 5,793,000 Combustion/Heat Exchanger Program 630,000

OFFICE OF TRANSPORTATION TECHNOLOGIES $24,249,000 Transportation Materials Technology 24,249,000 Automotive Materials Technology 17,483,000 Propulsion Systems Materials 5,483,000 Lightweight Vehicle Materials Technology 12,000,000 Electric Drive Vehicle Technologies 3,397,000 Advanced Battery Programs 2,997,000 Fuel Cell Materials 400,000 Heavy Vehicle Materials Technology 3,369,000

OFFICE OF UTILITY TECHNOLOGIES $38,810,000 Office of Solar Energy Conversion 18,460,000 Photovoltaic Energy Technology Division 18,460,000 Office of Geothermal Technologies 600,000 Office of Energy Management 19,750,000 Advanced Utility Concepts Division 19,750,000 High Temperature Superconductivity for Electric Systems 19,750,000

7 FY 1997 Budget Summary for DOE Materials Activities

FY 1997 BUDGET SUMMARY FOR DOE MATERIALS ACTIVITIES (continued)

FY 1997

OFFICE OF ENERGY RESEARCH $431,936,392 Office of Basic Energy Sciences 344,107,192 Division of Materials Sciences 332,060,000 Division of Chemical Sciences 5,143,000 Division of Engineering and Geosciences 6,904,192 Engineering Sciences Research 3,946,973 Geosciences Research 2,957,219 Office of Computational and Technology Research 76,651,200 Division of Advanced Energy Projects and Technology Research 76,651,200 Laboratory Technology Research (LTR) Program 8,062,000 Advanced Energy Projects Program 5,640,000 Small Business Innovation Research Program 58,849,611 Small Business Technology Transfer Program 4,099,589 Office of Fusion Energy Sciences 11,178,000

OFFICE OF ENVIRONMENTAL MANAGEMENT $6,870,939

OFFICE OF NUCLEAR ENERGY, SCIENCE AND TECHNOLOGY $65,080,000 Office of Engineering and Technology Development 2,080,000 Space and National Security Programs 2,080,000 Office of Naval Reactors 63,000,000'

OFFICE OF CIVILIAN RADIOACTIVE WASTE MANAGEMENT $15,400,000

OFFICE OF DEFENSE PROGRAMS The Weapons Research, Development and Test Program $96,633,600 Sandia National Laboratories 23,183,600 Lawrence Livermore National Laboratory .20,250,000 Los Alamos National Laboratory 53,200,000

OFFICE OF FOSSIL ENERGY $4,914,000 Office of Advanced Research 4,914,000 Fossil Energy AR&TD Materials Program 4.914.000

TOTAL $717.581.436

'This excludes $47 million for the cost of irradiation testing in the Advanced Test Reactor (ATR).

8 FY 1997 Budget Summary for DOE Materials Activities

The distribution of these funds between DOE laboratories, private industry, academia and other organizations is listed below.

Office of Building Technology, State and $1,090,000 $0 $0 $0 $1,090,000 Community Programs

TechnologiesOfiechnofogindstl $13,722,000 $15,617,208 $3,258,297 $0 $32,597,505

Technorlogies $17,925,000 $2,940,000 $3,084,000 $300,000 $24,249,000 Office of Utility $29,310,000 $9,500,000 $0 $0 $38,810,000

Office of Energy Research $331,608,800 $65,199,200 $34,486,863 $641,529 $431,936,392

Office of Environmental $4,965,355 $250,000 $1,448,252 $207,332 $6,870,939

Office of Nuclear Energy, $65,080,000 $0 $0 $0 $65,080,000 Science and Technology .... ______.____ ~$6 Office of Civilian Taecholgytv aste ad$15,400,000 $0 $0 $0 $15,400,000 Management Office of Defense Programs $96,633,600 0 $0 $00 $0$96,633,600 Office of Fossil Energy $3,979,000 $558,000 $357,000 $20,000 $4,914,000

Totals $579,713,75 $$94,064,408 $42,634,412 $1,168,861 $717,581,436

9 Office of Energy Efficiency and Renewable Energy

OFFICE OF ENERGY EFFICIENCY AND RENEWABLE ENERGY

The Office of Energy Efficiency and Renewable Energy seeks to develop the technology needed for the Nation to use its existing energy supplies more efficiently, and for it to adopt, on a large scale, renewable energy sources. Toward this end, the Office conducts long-term, high-risk, high-payoff R&D that will lay the groundwork for private sector action.

A number of materials R&D projects are being conducted within the Energy Efficiency and Renewable Energy program. The breadth of this work is considerable, with projects focusing on coatings and films, ceramics, solid electrolytes, elastomers and polymers, corrosion, materials characterization, transformation, superconductivity and other research areas. The level of funding indicated refers only to the component of actual materials research.

10 Office of Energy Efficiency and Renewable Energy

The Office of Energy Efficiency and Renewable Energy conducts materials research in the following offices and divisions: FY 1997

OFFICE OF BUILDING TECHNOLOGY, STATE AND COMMUNITY PROGRAMS $ 1,090,000 Office of Building Systems 1,090,000

OFFICE OF INDUSTRIAL TECHNOLOGIES $32,597,505 Office of Industrial Strategies 10,398,309 Aluminum Vision Team 5,071,000 Forest Products Vision Team 1,084,012 Steel Vision Team 455,000 Glass Vision Team 1,228,000 Metal Casting Vision Team 2,560,297 Office of Crosscut Technologies 22,199,196 Advanced Turbine System (ATS) Program 7,350,000 Continuous Fiber Ceramic Composites (CFCC) Program 8,400,000 Advanced Industrial Materials (AIM) Program 5,793,000 Combustion/Heat Exchanger Program 656,196

11 Office of Building Technology, State and Community Programs

OFFICE OF BUILDING TECHNOLOGY, STATE AND COMMUNITY PROGRAMS

FY 1997

Office of Building Technology. State and Community Programs - Grand Total $1,090,000

Office of Building Systems $1,090,000

Materials Properties. Behavior. Characterization or Testing $1,090,000

Development of Non-HCFC Foam Insulations 250,000 Evacuated Panel Insulation 250,000 Existing Materials Performance 110,000 Development of Sustainable Insulations 250,000 Standard Procedures for Measuring Solar Reflectivity of Roofs and Pavements 230,000

12 Office of Building Technology, State and Community Programs

OFFICE OF BUILDING TECHNOLOGY, STATE AND COMMUNITY PROGRAMS

OFFICE OF BUILDING SYSTEMS 2. EVACUATED PANEL INSULATION $250,000 The goal of this Office is to provide a scientific and DOE Contact: Arun Vohra, (202) 586-2193 technical basis (including model standards) for reducing ORNL Contact: Ken Wilkes, (423) 574-5931 the use of energy in residential and commercial buildings by 35 percent by the year 2000 from that used This project is for the development of an advanced in 1975, while maintaining existing levels of human technology super insulation concept. A filler layer of comfort, health and safety. The Division's primary powder, fiber or foam is encapsulated in a vacuum objectives are to support research that advances the barrier and a soft vacuum is drawn on the powder filler. scientific and technical options for increased energy Current technology produces R-30 and R-40 per inch efficiency in buildings, to promote the substitution of panels. More efficient and/or less expensive fillers and abundant fuels for scarce fuels in buildings, and to longer life encapsulating materials are being developed. promulgate standards for increased efficiency of energy Initial applications are to the walls and doors of use. To accomplish a portion of this, the Building refrigerators/freezers. Other applications, including Materials program seeks to: (1) develop new and building envelopes, are being developed. improve existing insulating materials; (2) develop and verify analytical models that are useful to building Keywords: Insulation, Vacuum, Heat Transfer, designers and researchers for predicting the thermal Refrigerators performance characteristics of materials; (3) develop methods for measuring the thermal performance 3. EXISTING MATERIALS PERFORMANCE characteristics; and (4) provide technical assistance and $110,000 advice to industry and the public. The DOE contact is DOE Contact: Arun Vohra, (202) 586-2193 Arun Vohra, (202) 586-2193. LBL Contact: Dariush Arasteh, (510) 486-6844

MATERIALS PROPERTIES, BEHAVIOR, This project is for the development of accurate and CHARACTERIZATION OR TESTING reproducible data for use by the building materials community, improved test procedures to determine the 1. DEVELOPMENT OF NON-HCFC FOAM thermal properties of existing, as well as advanced, INSULATIONS insulations, interacting with the building materials $250,000 research community, manufacturers, trade associa- DOE Contact: Arun Vohra, (202) 586-2193 tions, professional societies, compliance groups and ORNL Contact: Ken Wilkes, (423) 574-5931 local government, and making and disseminating recommendations on appropriate usage of thermal This project is for the development of foam insulations insulation to conserve energy. that use alternative blowing agents as drop-in replacements for the CFC blowing agents that were Keywords: Insulation, Buildings previously used in the manufacture of foam insulation products and for the HCFC blowing agents that are 4. DEVELOPMENT OF SUSTAINABLE currently being used. Prototype foam insulation boards INSULATIONS and refrigerator panels were sent to ORNL for testing $250,000 and evaluation. Tests are being conducted to determine DOE Contact: Arun Vohra, (202) 586-2193 thermal properties and aging characteristics. Models are ORNL Contact: Ken Wilkes, (423) 574-5931 being developed for aging processes, including the effects of facing materials. This project is for the identification and development of low-cost sustainable insulation materials and systems Keywords: CFC, Foam Insulation, Insulation for use in the building envelope. A survey and Sheathing, Roofs, HCFC, Refrigerators evaluation of information is being conducted to identify potentially applicable materials, known properties, deficiencies in knowledge of properties, level of availability, climatic and geographic range of applicability, environmental benefits and concerns, and costs of materials, transportation and any required treatment or processing. Laboratory evaluations of

13 Office of Building Technology, State and Community Programs candidate materials will focus on thermal performance and other characteristics.

Keywords: Insulation, Sustainability, Building Envelope

5. STANDARD PROCEDURES FOR MEASURING SOLAR REFLECTIVITY OF ROOFS AND PAVEMENTS $230,000 DOE Contact: Mark Decot, (202) 586-6501 LBL Contact: Hashem Akbari, (510) 486-4287 ORNL Contact: Jeff Christian, (423) 574-5207

Reflectivity of exterior building materials used for pavement and roofing has been demonstrated to affect heating and cooling costs in buildings where they are applied. The reflectivity of these surfaces also has an effect on creating urban heat islands where ambient air temperature has an additional indirect effect on heating and cooling costs in buildings. Exterior surface reflectivity also has an effect on urban smog formation and indoor air quality. This research on procedures for measuring reflectivity and characterizing effects or urban heat islands is being conducted in cooperation with ASTM, the Lawrence Berkeley Laboratory, Oak Ridge National Laboratory, Cool Roof Rating Council, Environmental Protection Agency and other Cool Communities partners.

Keywords: Solar Reflectivity, Building Materials, Heat Islands, Smog, Energy Efficiency

14 Office of Industrial Technologies

OFFICE OF INDUSTRIAL TECHNOLOGIES

FY 1997

Office of Industrial Technologies - Grand Total $32,597,505

Office of Industrial Strategies $10,398,309

Aluminum Vision Team $ 5,071,000

Device or Component Fabrication. Behavior or Testing $ 1,935,000

Aluminum Bridge Deck System 360,000 InLine Sensors for Electrolytic Aluminum Cells 254,000 Detection and Removal of Molten Salts from Molten Aluminum 294,000 High-Efficiency, High-Capacity, Low-NO, Aluminum Melting Using Oxygen- Enhanced Combustion 527,000 Technology for Converting SPL to Useful Glass Fiber Products 500,000

Materials Properties. Behavior. Characterization or Testing $ 970,000

Molten Aluminum Explosion Prevention 100,000 Innovative Vertical Flotation Melter 300,000 Aluminum Pilot Cell 570,000

Materials Preparation. Synthesis. Deposition. Growth or Forming $ 2,166,000

Recycling Aluminum Salt Cake 500,000 Wettable Ceramic-Based Drained Cathode Technology for Aluminum Electrolysis Cells 666,000 Aluminum Spray Forming 1,000,000

Forest Products Vision Team $ 1,084,012

Materials Properties. Behavior. Characterization or Testing $ 1,084,012

Corrosivity Monitoring of Kraft Recovery Boilers 1,084,012

Steel Vision Team $ 455,000 Device or Component Fabrication. Behavior or Testing $ 455,000

Intermetallic Alloy Development Related to the Steel Industry 455,000

Glass Vision Team $ 1,228,000

Materials Preparation. Synthesis. Deposition. Growth or Forming $ 364,000

Chemical Vapor Deposition Ceramic Synthesis 364,000

Materials Properties. Behavior. Characterization or Testing $ 864,000

Development of Improved Refractories 364,000 Synthesis and Design of MoSi2 Intermetallic Materials 500,000

15 Office of Industrial Technologies

OFFICE OF INDUSTRIAL TECHNOLOGIES (Continued)

FY 1997

Office of Industrial Strategies (continued)

Metal Casting Vision Team $2,560,297

Materials Preparation. Synthesis. Deposition. Growth or Forming $1,333,502

Assessment of Fast Shot Transition Point on Filling Patterns and Casting Quality for Pressure Die Castings 122,000 Unconventional Methods for Yield Improvement through Directional Solidification in Steel Castings 200,000 Plasma Refining Process Development 176,000 Heat Transfer at the Mold/Metal Interface in Permanent Mold Casting of Aluminum Alloys 155,921 Clean Cast Steel: 1) Flow of Steel in Gating Systems; 2) Control Ladle Temperature 220,000 Thin Section Steel Castings 88,581 Clean Metal Processing (Aluminum) 169,000 Advanced Lost Foam Casting Technology 202,000

Materials Properties. Behavior. Characterization or Testing $1,053,185 High Speed Milling and Pulsed ECM 126,000 Design Parameters for Lead Free Copper-Based Engineering Alloys in Permanent Molds 88,000 Process Parameters for Lead-Free Copper-Based Engineering Alloys in Permanent Molds 61,000 Impurity Limits in Aluminum Bronzes 57,000 Characterization of and Procedures to Eliminate Macro-Inclusion During Foundry Processing 43,000 Determination of Residual Stress and Softening Effects on the Life of Die Casting Dies 108,000 Development of Database Design Rules for Cast, High Alloy Steel Components 79,000 Semi-solid Metals Processing Consortium 54,000 Mechanical Properties Structure Correlation for Commercial Specifications of Cast Particulate Metal Matrix Components 46,000 Mechanical Properties of Squeeze and Semi-solid Cast A356 46,000 Ferrite Measurements in Duplex Stainless Steel Castings 50,000 Technology for the Production of Clean, Thin Wall, Machinable Gray and Ductile Iron Castings 201,853 Relationship Between Casting Distortion, Mold Filling and Interfacial Heat Transfer in Sand Molds 93,332

Device or Component Fabrication. Behavior or Testing $ 173,610

Intelligent Control of the Cupola Furnace 173,610

16 Office of Industrial Technologies

OFFICE OF INDUSTRIAL TECHNOLOGIES (Continued)

FY 1997

Office of Crosscut Technologies $22,199,196

Advanced Turbine System (ATS) Program $ 7,350,000

Device or Component Fabrication. Behavior or Testing $ 4,000,000

Ceramic Components for Stationary Gas Turbines in Cogeneration Service 4,000,000

Materials Properties. Behavior. Characterization or Testing $ 350,000

Long-Term Testing of Ceramic Components for Stationary Gas Turbines 350,000

Materials Preparation. Synthesis. Deposition. Growth or Forming $ 3,000,000

ATS Materials Base Technology Support 3,000,000

Continuous Fiber Ceramic Composites (CFCC) Program $ 8,400,000

Materials Preparation. Synthesis. Deposition. Growth or Forming $ 6,400,000

CFCC Program - Industry Tasks 6,400,000

Materials Properties. Behavior. Characterization or Testing $ 2,000,000

Continuous Fiber Ceramic Composites (CFCC) Supporting Technologies 2,000,000

Advanced Industrial Materials (AIM) Program $ 5,793,000

Materials Preparation. Synthesis. Deposition. Growth or Forming $ 3,302,000

Intermetallic Alloy Development and Technology Transfer of Intermetallic Alloys 515,000 Development of Weldable, Corrosion Resistant Iron-Aluminide Alloys 290,000 Composites and Coatings Through Reactive Metal Infiltration 443,000 Conducting Polymers: Synthesis and Industrial Applications 250,000 Membrane Systems for Efficient Separation of Light Gases 309,000 Microwave and Plasma Processing 275,000 Uniform Droplet Processing 440,000 Advanced Materials/Processes 780,000

Materials Properties. Behavior. Characterization or Testing $ 1,375,000

Materials for Recovery Boilers 940,000 Metals Processing Laboratory User (MPLUS) Center 435,000

Device or Component Fabrication. Behavior or Testing $ 610,000

Gel Casting Technology 110,000 Microwave Joining of SiC 110,000 Selective Inorganic Thin Films 350,000 High Temperature Particle Filtration Technology 40,000

17 Office of Industrial Technologies

OFFICE OF INDUSTRIAL TECHNOLOGIES (Continued)

FY 1997

Office of Crosscut Technologies (continued)

Advanced Industrial Materials (AIM) Program (continued)

Materials Structure and Composition $506,000

Metallic and Intermetallic Bonded Ceramic Composites 165,000 Processing of Polymers in a Magnetic Field 341,000

Combustion/Heat Exchanger Program $656,196

Materials Properties. Behavior. Characterization or Testing $630,000

Advanced Heat Exchanger Material Technology Development 630,000

Device or Component Fabrication. Behavior or Testing $ 26,196

High Pressure Heat Exchanger System (HiPHES) Energy Production 0 High Pressure Heat Exchanger System (HiPHES) for Ethylene Production 26,196

18 Office of Industrial Technologies

OFFICE OF INDUSTRIAL TECHNOLOGIES

The mission of the Office of Industrial Technologies (OIT) is to support the development and deployment of advanced energy efficiency, renewable energy and pollution prevention technologies for industrial applications. OIT's R&D portfolio is driven by needs the Industries of the Future: chemicals, forest products, steel, aluminum, metalcasting and glass. These industries account for over half of all manufacturing energy use and account for 75 to 90 percent of most manufacturing wastes.

The Industries of the Future strategy uses industry-developed visions and technology roadmaps to outline the technology that will be needed in order to reach their goals. Through this process, government-funded research is brought to a sharp focus to benefit U.S. industry. OIT's R&D portfolio includes process R&D directly related to specific industries of the future and crosscutting R&D which is applicable to multiple industries. Technology Access programs assist in delivering state-of-the-art and emerging technologies to industry customers.

OFFICE OF INDUSTRIAL STRATEGIES environmental fatigue characterization of composite paving surfaces. The Industries of the Future (specific) mechanism cost-shares with industry and other organizations Keywords: Aluminum, Bridge Decks, Extrusions technology development identified in industry-wide developed visions and roadmaps. These technologies, 7. INLINE SENSORS FOR ELECTROLYTIC specific to industry processes, are chosen based on ALUMINUM CELLS their ultimate impact on energy and waste reduction, $254,000 high priority and high risk to meet roadmap targets, DOE Contact: Sara Dillich, (202) 586-7925 widespread industry applicability and pre-competitive ORNL Contact: Jack Young, (423) 5744922 nature. Materials research addresses the need for industrial processes to run at increased temperatures Through an existing Cooperative Research and with longer service lives, reduced downtime, and lower Development Agreement (CRADA) with industrial capital costs. partners, Oak Ridge National Laboratory (ORNL), will develop a sensor for use in both conventional and ALUMINUM VISION TEAM - The DOE Aluminum advanced inert anode aluminum production cells. Fiber Team leader is Hank Kenchington, (202) 586-1878 optic probes and laser-based Raman spectra analytical techniques are being investigated to measure soluble DEVICE OR COMPONENT FABRICATION, alumina in cryolite. Sensors for measurement of bath BEHAVIOR OR TESTING ratio and bath temperature will be investigated in future stages of the project. Dynamic process and thermal 6. ALUMINUM BRIDGE DECK SYSTEM modeling will be developed in concert with these $360,000 sensors to enable utility power load leveling through DOE Contact: Sara Dillich, (202) 586-7925 thermal cycling of the production cells without loss of ORNL Contact: Wayne Hayden, (423) 5746936 productivity. A Raman cell for laboratory use has been designed and fabricated. Identifying a material that can The project objective is to develop and refine a bridge endure cryolite melts is another barrier to developing a deck panel system consisting of aluminum multi-void reliable sensor. Thus, research to date has focused on extrusions joined to make panel sections. The desired the development of coating materials for a silica probe, results are to renovate deficient bridges and build new and three coating materials (CVD diamond, hot-pressed bridges throughout the U.S. using the aluminum bridge PBN and TBN) that appear to survive in cryolite melts deck system. The project is being cost-shared under a during preliminary testing have been identified. Cooperative Research and Development Agreement Investigations are continuing into probe tip fabrication between Reynolds Metals Company, Inc. and Oak and coating, immersion tests in molten salts, and Ridge National Laboratory (ORNL). The experimental Raman characterization of cryolite. plan has been established and ORNL is conducting work related to panel welding and NDE procedures, Keywords: Sensor, Raman Probe, Fiber Optic Probe, alternative welding procedures for onsite repairs, fatigue Cryolite, Alumina characterization of mechanically fastened aluminum joints, wear testing of composite paving surfaces, and

19 Office of Industrial Technologies

8. DETECTION AND REMOVAL OF MOLTEN burner at the optimum 35-50 percent combined total SALTS FROM MOLTEN ALUMINUM oxidizer stream using both the product and the exhaust $294,000 streams from the VSA. The second phase includes the DOE Contact: Sara Dillich, (202) 586-7925 integration of the VSA to meet the average demand through proprietary storage, versus the current, less In a one-year effort beginning in September 1997, Selee efficient practice of sizing to meet peak demand. The Corporation and Alcoa Technical Center will conduct a successful demonstration of this project will provide the program to detect and reduce chloride salts in molten U.S. aluminum industry with a cost-effective, aluminum. Selee Corporation has invented a simple energy-efficient, environmentally-friendly modification electrical probe that senses the presence of salts in for current melting furnaces. molten aluminum. Although consistent results have been seen in laboratory and plant tests, this salt Keywords: Aluminum Melting, Combustion, Burner detector needs to be calibrated. That is, its response must be correlated to the specific level of salts in the 10. TECHNOLOGY FOR CONVERTING SPL TO metal so that the response can be accurately USEFUL GLASS FIBER PRODUCTS interpreted. Selee has also invented a filter which $500,000 selectively removes liquid salts from the liquid metal. DOE Contact: Sara Dillich, (202) 586-7925 This has been demonstrated in laboratory tests, but tests in real casting conditions must be carried out to Vortec Corporation, assisted by Alumax Primary determine efficiency and capacity of the filter. Using the Aluminum Corp., Hoogovens Technical Services, Inc., experimental casting facility at the Alcoa Technical and the New York State College of Ceramics at Alfred Center, these two devices will be exposed to various University, will perform a pilot-scale experimental levels of chlorine and metal flow rates using commercial testing project to evaluate the feasibility of converting alloys. The response of the probe will be correlated with SPL (spent potliner) from aluminum smelting plants to chlorine levels over a wide range of conditions. At the commercial quality glass fiber and aluminum fluoride same time, the efficiency of the salt filter will be products using Vortec's Cyclone Melting System assessed. By monitoring the efficiency of the filter as a (CMSTm) technology. The project, initiated in September function of chlorine and time in casting, the adsorptive 1997, will be performed during a 20-month period and capacity of filter media can be determined. The goal of will include the following activities: this project is to develop and demonstrate the technology at commercial-scale in one year. 1. Design, fabrication, and installation of pilot-scale Commercial implementation by the domestic aluminum glass fiberizing and flue gas filtration and analysis industry should be realized soon after, probably within equipment into Vortec's existing pilot-scale CMST another year. testing facility 2. Pilot-scale SPL vitrification test to produce glass Keywords: Molten Aluminum, Salts, Filter, Probe fibers 3. Testing and analysis of the fibers from the 9. HIGH-EFFICIENCY, HIGH-CAPACITY, LOW-NOx pilot-scale test with respect to commercial quality ALUMINUM MELTING USING OXYGEN- specifications ENHANCED COMBUSTION 4. Testing and analysis of fibers with respect to $527,000 human health considerations DOE Contact: Ramesh Jain, (202) 586-2381 5. Sampling and analysis of flue gas from the pilot-scale CMS TM during testing Air Products & Chemicals, Inc. along with Argonne 6. Preliminary design of a commercial-scale air National Laboratory, Roth Brothers, and Brigham Young pollution system for aluminum fluoride production. University will develop and demonstrate a novel, high-efficiency, high-capacity, low-NOx, combustion Keywords: Potliner, Aluminum Smelting, Glass Fiber, system integrated with an innovative low-cost, on-site Aluminum Fluoride vacuum-swing- absorption (VSA) oxygen generation. This integrated burner/oxygen supply system will offer enhanced productivity, high-energy efficiency, low operating costs, and low NOx emissions.

This two-year project, which began in September 1997, will be conducted in two phases. The first phase includes the design and construction of a low-NOx

20 Office of Industrial Technologies

MATERIALS PROPERTIES, BEHAVIOR, VFM, where particles of varying sizes and surface areas CHARACTERIZATION OR TESTING are kept in suspension at different levels of the melter, designed with varying velocities to achieve the desired 11. MOLTEN ALUMINUM EXPLOSION drag forces. The scrap pieces reach an equilibrium in PREVENTION which the scrap weight equals the gas drag force, and $100,000 the scrap is suspended for 15 to 30 seconds, allowing DOE Contact: Ramesh Jain, (202) 586-2381 sufficient residence time for it to melt. The melting ORNL Contact: Rusi P Taleyarkhan, 423 5764735 particles experience changes in their aerodynamic shape until they reach the liquid state and fall into a The goal of this project is to improve industry's molten metal bath. This process also has applications understanding of the conditions that trigger aluminum- in the glass and steel industries. water explosions and the reasons and extent to which certain coatings prevent those explosions. Project Keywords: Floatation Melter, Aluminum Scrap partners (ORNL, The Aluminum Association, Alcoa) will achieve this goal through developing a basic under- 13. ALUMINUM PILOT CELL standing of entrapment of heat transfer over submerged $570,000 coated and uncoated surfaces. Partners have designed DOE Contact: Sara Dillich, (202) 586-7925 and developed the Steam Explosion Triggering Studies (SETS) facility, an experimental test site where the The Department of Energy, Office of Industrial fundamental issues of explosions will be investigated Technologies is currently sponsoring a project with the with emphasis on triggering events. Solid tungsten, an Aluminum Company of America (Alcoa) to demonstrate, element that has thermophysical properties similar to through pilot cell tests, viability of an advanced retrofit those of liquid aluminum, will be used during the technology for alumina reduction based on inert, cermet experiments to allow the apparatus to be instrumented anodes and wettable TiB2-G cathodes. Phase I of the and the phenomena associated with the breakdown of Alcoa project developed a retrofit commercial cell steam film and triggering investigated without the conceptual design and assessed its economic and hazards associated with experiments performed with environmental impact. Phase II is conducting tests in a large amounts of liquid aluminum. The initial coping pilot-scale cell and an evaluation of lower cost/higher assessment and the preliminary testing to verify the quality fabrication of inert anodes. The objectives of project's approach and direction have been completed. Phase II are to construct, operate, and autopsy two In addition, feedback has been provided to industry pilot-scale cells; the first based on best available testing programs. Suppression capability data for technology and the second optimized as a result of the various coatings with different curing times and their knowledge gained from the first. These tests will also application criteria has been obtained, as well as the feature Bayer process improvements, and advanced cell suppression capability data for various coatings based design and control systems. Anodes will be fabricated on the evolution of non-condensable gases and by isostatic pressing and sintering of metal and oxide wettability. powders. Innovative fabrication methods for anode-collector bar assembly are also being Keywords: Explosions, Molten Aluminum, Water investigated. 12. INNOVATIVE VERTICAL FLOATATION MELTER Keywords: Alumina Reduction, Aluminum Production, $300,000 Inert Anode, Wettable Cathodes DOE Contact: Ramesh Jain, (202) 586-2381 MATERIALS PREPARATION, SYNTHESIS, The vertical floatation melter (VFM) is being developed DEPOSITION, GROWTH OR FORMING by Energy Research Company, Gillespe and Powers, IMCO, and Stein, Atkinson and Stordy with support 14. RECYCLING ALUMINUM SALT CAKE from the Office of Industrial Technologies. This $500,000 technology represents a significantly cleaner and more DOE Contact: Sara Dillich, (202) 586-7925 efficient alternative for processing aluminum scrap. In ANL Contact: John Hryn, (630) 252-5894 the new process, the scrap is first dried and de-coated in a rotary kiln dryer that completely removes organics Salt cake recovery is the most energy and cost intensive such as oil, paint, and plastics. The heat content of the unit operation in the recovery of salt cake constituents. organics volatizing from the scrap will supply In this project, Argonne National Laboratory (ANL) is supplementary heat to the de-coater. The dried and developing a salt recovery process based on electrode-coated scrap is then melted in the opposed flow dialysis (ED). Laboratory scale experiments and

21 Office of Industrial Technologies economic analysis has indicated that, for conditions 16. ALUMINUM SPRAY FORMING consistent with salt cake recycling, the ED technology is $1,000,000 more cost-effective for salt recovery than alternative DOE Contact: Sara Dillich, (202) 586-7925 technologies (e.g., evaporation with vapor recom- pression). Increasing the market value of NMP is This project, conducted by the Aluminum Company of critical for cost-effective salt cake recycling. Impurities America (Alcoa), will translate current bench-scale constitute about 10 percent of NMP and lower its market spray forming technologies into a cost-effective process value. Research is investigating hydrometallurgical for the replacement of the energy-intensive ingot casting processes to purify NMP, since higher NMP purity method. A unique linear spray nozzle system has been results in higher market value for refractory aggregate designed which has the potential for achieving the and other potential alumina markets. Markets which will desired production rates of 1500 to 3000 Ib./hr/in in a require lower development costs, such as alternative single pass operation. Other processing targets include alumina units for the blast furnace in ironmaking, are ±2 percent profile flatness, less than 1-inch edge also being explored. trimming; surface porosity of less than 4 percent not interconnected, and overspray less than 5 percent. Keywords: Aluminum, Salt Cake, Recycling, Thermomechanical processing studies, microstructural Electrodialysis characterization of deposits, and mathematical and numerical modeling are in progress. Investigations are 15. WETTABLE CERAMIC-BASED DRAINED focusing on as-sprayed microstructure and thermo- CATHODE TECHNOLOGY FOR ALUMINUM mechanical properties of automotive alloy 6111. An ELECTROLYSIS CELLS Advanced Development Unit, capable of operating in $666,000 both an experimental and a semi-production mode, is DOE Contact: Sara Dillich, (202) 586-7925 being designed and constructed to investigate the commercial viability of the spray forming process to Reynolds Metals Company, Kaiser Mead, and produce aluminum sheet. The unit will be used to Advanced Refractory Technologies (ART) will determine costs as well as processing and safety collaborate to develop and evaluate ceramic-based procedures for steady state operations. materials, technology, and the necessary engineering packages to retrofit existing reduction cells as a means Keywords: Aluminum, Spray Forming, Sheet to improve the performance of the Hall Heroult cell. ART will produce TiB2-based tiles or coatings that will be FOREST PRODUCTS VISION TEAM - The DOE Forest used as the 'drained" lining in two 70 kA prebake cells. Products team leader is Valri Robinson, (202) 586-0937 The durability of the candidate materials and the performance of the drained cathode design will be MATERIALS PROPERTIES, BEHAVIOR, evaluated during a one-month test using 12 kA pilot CHARACTERIZATION, OR TESTING reduction cells. This four-year project, initiated in September 1997, will include the following activities: 17. CORROSIVITY MONITORING OF KRAFT RECOVERY BOILERS 1. Development and evaluation of candidate TiB2- $1,084,012 carbon materials (tiles and coating) DOE Contact: Charles A. Sorrell, (202) 586-1514 2. Development and evaluation of proprietary carbon IPST Contact: Preet Singh, (404) 894-6641 materials 3 Development of the drained cathode design The focus of this project is to develop an extensive 4. Evaluation of the best candidate materials and the corrosion kinetics database as well as a device to drained cathode design in the 12 kA pilot cell measure conditions which control corrosion in an 5. Design and construction of a 70 kA prebake cell operating recovery boiler. The benefit of such an retrofitted with a drained cathode using approach will allow operators to predict or explain the TiB2-based and or the proprietary materials impact of decisions prior to damaging boiler 6. Startup and operation of two 70 kA prebake cells components. The project will be divided into four retrofitted with a drained cathode and TiB2 and or phases. Phase I will establish the feasibility of the the proprietary materials project concept, Phase II will involve detailed studies on the most promising candidates for corrosion Keywords: Cathode, Aluminum Production, Titanium measurements, Phase III consists of small scale Diboride experiments conducted in a laboratory furnace to test the efficacy of the measurement system developed in Phase II, and in the final Phase IV, the measurement

22 Office of Industrial Technologies device and corrosion probes will be installed in a GLASS VISION TEAM - The DOE Glass team leader is operating boiler for comparison. Theo Johnson, (202) 586- 6937

Keywords: Recovery Boilers, Corrosion, Pulp and Paper MATERIALS PREPARATION, SYNTHESIS, DEPOSITION, GROWTH OR FORMING STEEL VISION TEAM - The DOE Steel team leader is Scott Richlen, (202) 586 - 2078 19. CHEMICAL VAPOR DEPOSITION CERAMIC SYNTHESIS DEVICE OR COMPONENT FABRICATION, $364,000 (funded by the OIT Glass Vision team) BEHAVIOR OR TESTING DOE Contact: Charles A. Sorrell, (202) 586-1514 Sandia National Laboratories - Livermore Contact: 18. INTERMETALLIC ALLOY DEVELOPMENT M. D. Allendorf, (415) 294-2895 RELATED TO THE STEEL INDUSTRY $455,000 Comprehensive models, including detailed gas-phase DOE Contact: Charles A. Sorrell, (202) 586-1514 and surface chemistry coupled with reactor fluid ORNL Contacts: M. L. Santella, (423) 574-4805, mechanics, are required to optimize and scale-up V. K. Sikka, (423) 574-5112, and P.Angelini chemical vapor deposition +(CVD) processes. The (423) 574-4565 objective of this project is to use the unique diagnostic and modeling capabilities at the Sandia National The objective of this project is to develop and apply the Laboratories - California to understand and develop new excellent oxidation and carburization resistance and techniques for chemical vapor deposition (CVD). A higher strength of intermetallic alloys including nickel research reactor, originally constructed with DOE-OIT aluminides (Ni3AI) to Steel industry related manufac- funding, is being used to determine identities and turing applications. Progress in bringing technologies to amounts of gaseous phase species present during CVD. development and commercialization in FY 1997 focused Research efforts are focused on development of CVD on furnace transfer rolls for use in the heat treating of processes for oxide fiber-preforms and plate glass steel slabs: 1) Two types of furnace roll designs have surfaces for the improvement of properties. In FY1997 a been fabricated and are being tested at Bethlehem CRADA was developed with Libby- Owens-Ford Co. on Steel; both types utilize a welded connection between a developing new CVD techniques for depositing coatings trunnian and a roll body, 2) Technology for joining thick on glass. With respect to this project: (1) a database sections of Ni3AI to dissimilar metals was developed, was developed of thermodynamic properties for the and two rolls are being tested utilizing HK or HP steel deposition of coatings on glass, (2) experimental trunnians welded to Ni3AI roll bodies, 3) After working techniques were developed for identifying reactions of with various companies on materials and process the glass-coating precursors, and (3) the kinetics of development of Ni3AI two companies have been several reactions were measured. In the task on licensed, including Alloy Engineering and Casting composite and the fiber coating efforts: (1) an analytical Company, Sandusky International to produce Ni3AI model was completed to predict deposition of coatings materials and components. on ceramic fiber preforms, and (2) a model to quantitatively predict boron nitride coating rates in Keywords: Nickel Aluminides, Processing, Steel, chemical reactors was optimized. Metalcasting, Aluminum, Heat Treating, Welding Keywords: Chemical Vapor Deposition, Gas-Phase Chemistry, Modeling, Fibers, Flat Glass

23 Office of Industrial Technologies

MATERIALS PROPERTIES, BEHAVIOR, radiant tube environment. This will be a 500 hour test at CHARACTERIZATION OR TESTING 1800°F under gas combustion conditions.

20. DEVELOPMENT OF IMPROVED Keywords: Composites, Intermetallics, Molydisilicides, REFRACTORIES Coatings $364,000 DOE Contact: Charles A. Sorrell, (202) 586-1514 METAL CASTING VISION TEAM - The DOE Oak Ridge National Laboratory Contact: Metalcasting team leader is Harvey Wong, A. A. Wereszczak (423) 574-7601, and (202) 586-9235 Peter Angelini (423) 574-4565 MATERIALS PREPARATION, SYNTHESIS, Refractories are critical for various industrial processes. DEPOSITION, GROWTH OR FORMING For example, glass melting furnaces are fabricated with various types of refractories which enable the furnaces 22. ASSESSMENT OF FAST SHOT TRANSITION to be operated at very high temperatures, and steel or POINT ON FILLING PATTERNS AND CASTING aluminum smelting and melting vessels are lined with QUALITY FOR PRESSURE DIE CASTINGS refractories. The goal of this project is to develop $122,000 improved refractories and to determine critical DOE Contact: Toni Mar6chaux, (202) 586-8501 mechanical and thermophysical and mechanical Principal Investigator: Jerald Brevick, Ohio State properties. In FY 1997, work was focused on University (614) 292-0177 determining high temperature creep and corrosion behavior of refractories for use in oxifuel fired glass The objective of this project is to evaluate common making furnaces. Partners in this activity include the approaches to cavity filling, compare the results of Oak Ridge National Laboratory, Alfred University's current software metal flow models with fluid flow Center for Glass Research (CGR) Satellite Center at the observed on high-speed video, and compare the University of Missouri-Rolla, and an industrial technical location, size and total volume of contained gas team representing glass and refractories manufacturers. porosity.

Keywords: Refractories, Glass, Furnace, Oxi-fuel, High Keywords: Metalcasting, Metal Flow Temperature, Mechanical Thermophysical, Properties, Corrosion 23. UNCONVENTIONAL METHODS FOR YIELD IMPROVEMENT THROUGH DIRECTIONAL 21. SYNTHESIS AND DESIGN OF MOS I2 SOLIDIFICATION IN STEEL CASTINGS INTERMETALLIC MATERIALS $200,000 $500,000 DOE Contact: Toni Mar6chaux, (202) 586-8501 DOE Contact: Charles A. Sorrell, (202) 586-1514 Principal Investigator: Christoph Beckermann, Los Alamos National Laboratory Contacts: University of Iowa, (319) 335-5681 J. J. Petrovic, (505) 667-0125 and Richard Castro (505) 667-5191 This project is designed to increase yield through the use of solidification software to simulate imposed The objective of this project is to develop MoSi2-based thermal gradients and evaluate their effect on yield. composites that will combine good room temperature fracture toughness with excellent oxidation resistance Keywords: Metalcasting, Metal Flow and high-temperature strength for industrial applications. Activities in FY 1997 included various major 24. PLASMA REFINING PROCESS DEVELOPMENT tasks. A CRADA with Johns Manville Corporation on the $176,000 use of MoSi 2 for glass industry applications is con- DOE Contact: Toni Marechaux, (202) 586-8501 tinuing. The corrosion behavior of MoSi2 materials in Principal Investigator: Carl Lundin, University of molten fiberglass has been initially evaluated, and is Tennessee, (423) 974-5310 similar to AZS refractory. Maximum corrosion rates occur at the glass-air interface. Efforts have been The objective of this project is to improve the weldability initiated with IGT to test MoSi2 materials in a gas and corrosion resistance of high alloy castings; to demonstrate reductive alloying in a plasma furnace to

24 Office of Industrial Technologies

minimize oxidation losses of chromium and other 28. CLEAN METAL PROCESSING (ALUMINUM) elements; and to decarburize stainless steels efficiently. $169,000 DOE Contact: Toni Marechaux, (202) 586-8501 Keywords: Metalcasting, Corrosion, Welding, Stainless Principal Investigator: Diran Apelian, Worcester Steel Polytechnic Institute, (508) 831-5992

25. HEAT TRANSFER AT THE MOLD/METAL The objective of this project is to investigate and INTERFACE IN PERMANENT MOLD CASTING develop implementable metal cleanliness assessment OF ALUMINUM ALLOYS methods, melt contamination avoidance, and $155,921 augmentation of the fundamental knowledge base of DOE Contact: Toni Marechaux, (202) 586-8501 phase separation technology. Principal Investigator Robert Pehlke, University of Michigan, (313) 764-7489 Keywords: Metalcasting, Aluminum, Phase Separation

The objective of this project is to achieve enhanced 29. ADVANCED LOST FOAM CASTING dimensional control in permanent mold castings, TECHNOLOGY decreased cycle time and accurate control of heat $202,000 transfer. It is designed to increase die life and enable Principal Investigator: Charles Bates, University. of thinner section sizes. Alabama - Birmingham, (205) 975-8011

Keywords: Metalcasting, Aluminum, Permanent Mold The objective of this project is to perform research to Casting advance the theory and application of lost foam casting including: making castings under vacuum; to extend the 26. CLEAN CAST STEEL: 1) FLOW OF STEEL IN technology to allow bronze and steel alloy casting; GATING SYSTEMS; 2) CONTROL LADLE coating improvements; and flow, fill and solidification TEMPERATURE experiments. $220,000 DOE Contact: Toni Marechaux, (202) 586-8501 Keywords: Metalcasting, Lost Foam Casting Principal Investigator: Charles Bates, University of Alabama - Birmingham, (205) 975-8011 MATERIALS PROPERTIES, BEHAVIOR, CHARACTERIZATION, OR TESTING The objective of this project is: (1) to evaluate the effect of the flow of steel in gatings systems on steel casting 30. HIGH SPEED MILLING AND PULSED ECM quality; (2) to evaluate the effect of ladle temperature $126,000 homogenization on steel casting quality. DOE Contact: Toni Marechaux, (202) 586-8501 Principal Investigator: Taylan Altan, Ohio State Keywords: Metalcasting, Steel, Gatings University

27. THIN SECTION STEEL CASTINGS The objective of this project is to determine the $88,581 influence of HSM and PECM on residual stresses in the DOE Contact: Toni Mar6chaux, (202) 586-8501 die surface and its resistance to thermal fatigue and to Principal Investigator: Robert C. Voigt, develop guidelines for machining H-13 at a fully heat Pennsylvania State University, treated state. This will test the findings and determine (814) 863-7290 time and cost savings.

The objective of this project is to develop a fundamental Keywords: Metalcasting, Residual Stress, Machining understanding of the key technologies needed to develop lighter weight, thinner section steel castings.

Keywords: Metalcasting, Steel

25 Office of Industrial Technologies

31. DESIGN PARAMETERS FOR LEAD FREE 34. CHARACTERIZATION OF AND PROCEDURES COPPER-BASED ENGINEERING ALLOYS IN TO ELIMINATE MACRO-INCLUSION DURING PERMANENT MOLDS FOUNDRY PROCESSING $88,000 $43,000 DOE Contact: Toni Marechaux, (202) 586-8501 DOE Contact: Toni Mar6chaux, (202) 586-8501 Principal Investigator: Yemi Fasoyinu, Materials Principal Investigator Alan Cramb, Carnegie Technology Laboratory, (613) 996-0325 Mellon University, (412) 268-3517

The three year project objectives are to: determine the An inclusions atlas has been developed along with a set tensile, fracture toughness, impact and fatigue of standards to evaluate the cleanliness of steel properties of 12 copper-base alloys for use in more castings. The atlas has been made available on the demanding engineering applications; determine the dry world wide web. and lubricating sliding wear and slurry wear resistance; carry out corrosion studies (salt spray, atmospheric and Keywords: Metalcasting, Steel, Macro-inclusions marine); and determine pattern makers shrinkage and metal core taper allowance in permanent mold. 35. DETERMINATION OF RESIDUAL STRESS AND SOFTENING EFFECTS ON THE LIFE OF DIE Keywords: Metalcasting, Copper Alloys, Corrosion CASTING DIES $108,000 32. PROCESS PARAMETERS FOR LEAD-FREE DOE Contact: Toni Marechaux, (202) 586-8501 COPPER-BASED ENGINEERING ALLOYS IN Principal Investigator Jack Wallace, Case PERMANENT MOLDS Western Reserve University, (216) 368-4222 $61,000 DOE Contact: Toni Marechaux, (202) 586-8501 The objective of this project is to evaluate measurement Principal Investigator: Kumar Sadayappan, methods and develop ways of reducing losses in die life Materials Technology Laboratory, caused by softening of the steel and build-up of residual (613) 992-0741 stress.

The objective of this project is to develop process Keywords: Metalcasting, Residual Stress, Die Casting parameters such as evaluation of mold materials, improvement in casting fluidity, and grain refinement; to 36. DEVELOPMENT OF DATABASE DESIGN perform water and computer modeling to explain mold RULES FOR CAST, HIGH ALLOY STEEL filling and to evaluate high phosphorous lead-free brass COMPONENTS for plumbing applications. $79,000 DOE Contact: Toni Marechaux, (202) 586-8501\ Keywords: Metalcasting, Copper Alloys, Metal Flow Principal Investigator Martin Prager, Materials Properties Council, (215) 705-7694 33. IMPURITY LIMITS IN ALUMINUM BRONZES $57,000 The objective of this project is to develop design data, DOE Contact: Toni Mar6chaux, (202) 586-8501 screening tests and an atlas of micrographs. Principal Investigator: Yemi Fasoyinu, Materials Technology Laboratory, (613) 992-5475 Keywords: Metalcasting, Steel, Design Rules

The objective of this project is to study the effect of 37. SEMI-SOLID METALS PROCESSING impurity elements on the mechanical properties, CONSORTIUM weldability and heat treatment of two common $54,000 aluminum bronze alloys C95800 and C95400. The DOE Contact: Toni Marechaux, (202) 586-8501 impurity elements are Pb, Zn, Sn, Bi, Se, Si,Cr and Be. Principal Investigator: Diran Apelian, Worcester These will be added as single elements, and in two Polytechnic Institute, (508) 831-5992 element and three element combinations. The objective of this project is to characterize semi-solid Keywords: Metalcasting, Bronze, Mechanical Properties materials from a microstructure and rheology point of view, to better understand thixotropic flow behavior, and to develop. new and enhanced alloys.

Keywords: Metalcasting, Semi-Solid, Rheology

26 Office of Industrial Technologies

38. MECHANICAL PROPERTIES STRUCTURE machinability. It will then determine methods for CORRELATION FOR COMMERCIAL eliminating objectionable inclusions. SPECIFICATION OF CAST PARTICULATE METAL MATRIX COMPONENTS Keywords: Metalcasting, Gray Iron, Cast Iron, $46,000 -Inclusions DOE Contact: Toni Marechaux, (202) 586-8501 Principal Investigator Pradeep Rohadgi, 42. RELATIONSHIP BETWEEN CASTING University of Wisconsin - Milwaukee, DISTORTION, MOLD FILLING AND (414) 229-4987 INTERFACIAL HEAT TRANSFER IN SAND MOLDS The objective of this project is to establish procedures $93,332 for mechanical testing and structural characterization DOE Contact: Toni Marechaux, (202) 586-8501 and to provide comparative data and composites for Principal Investigator: Thomas Piwonka, quality assurance. University of Alabama - Tuscaloosa, (205) 348-1589 Keywords: Metalcasting, Metal Matrix Composite, Mechanical Testing The objective of this project is to determine the effect of interfacial heat transfer coefficients and gap formation 39. MECHANICAL PROPERTIES OF SQUEEZE AND in iron and aluminum sand mold castings on casting SEMI-SOLID CAST A356 dimensional accuracy. $46,000 DOE Contact: Toni Marechaux, (202) 586-8501 Keywords: Metalcasting, Iron, Aluminum, Sand Mold Principal Investigator Robert Aikin, Case Western Reserve University, (216) 368-4221 DEVICE OR COMPONENT FABRICATION, BEHAVIOR OR TESTING The objective of this project is to develop a mechanical properties database for A356 castings produced by the 43. INTELLIGENT CONTROL OF THE CUPOLA processes of squeeze casting and semi-solid casting. FURNACE $173,610 Keywords: Metalcasting, Aluminum, Squeeze Casting, DOE Contact: Toni Marechaux, (202) 586-8501 Semi-solid Casting Principal Investigator: Kevin Moore, Idaho State University, (208) 236-4188 40. FERRITE MEASUREMENTS IN DUPLEX STAINLESS STEEL CASTINGS The objective of this project is to develop a controller for $50,000 the cupola process using intelligent and conventional DOE Contact: Toni Marechaux, (202) 586-8501 control methods. Principal Investigator: Carl Lundin, University of Tennessee, (423) 974-5310 Keywords: Metalcasting, Cupola, Intelligent Control The objective of this project is to develop suitable OFFICE OF CROSSCUT TECHNOLOGIES methods for non-destructively measuring ferrite amounts for the surface of castings. The Office of Crosscut Technologies funds cost-shared research with industry and other organizations on Keywords: Metalcasting, Non-destructive Evaluation, technology development beneficial to and of high Stainless Steel priority for many industries. Power generation equipment, combustion equipment, advanced materials and 41. TECHNOLOGY FOR THE PRODUCTION OF sensors and controls are being pursued. The three CLEAN, THIN WALL, MACHINABLE GRAY AND planning units that fund materials research include the DUCTILE IRON CASTINGS Advanced Turbine Systems Program (ATS), Continuous $201,853 Fiber Ceramic Composites (CFCC) Program, Advanced DOE Contact: Toni Marechaux, (202) 586-8501 Industrial Materials (AIM) Program and the Combustion Principal Investigator Charles Bates, University of (Heat Exchanger) Program. Alabama - Birmingham, (205) 975-8011

This project will focus on identifying the phases and compounds which degrade properties and

27 Office of Industrial Technologies

ADVANCED TURBINE SYSTEM (ATS) PROGRAM fatigue, creep damage becomes the major consideration for both metallic and ceramic systems. This The Advanced Turbine Systems (ATS) Program will program characterizes the long-term properties of develop and demonstrate the next generation of gas advanced materials systems under the ATS materials/ turbines for both utility and industrial applications, manufacturing program. including cogeneration and combined heat and power. The goals of the ATS program are to improve the Keywords: Structural Ceramics, Creep Damage, Gas efficiency (15% increase) and environmental Turbines performance (80% reduction in emissions) of gas turbines while reducing the cost of electricity by 10%. MATERIALS PREPARATION, SYNTHESIS, The DOE program manager is Patricia Hoffman, DEPOSITION, GROWTH OR FORMING (202) 586-6074. 46. ATS MATERIALS BASE TECHNOLOGY DEVICE OR COMPONENT FABRICATION, SUPPORT BEHAVIOR OR TESTING $3,000,000 DOE Contact: Pat Hoffman, (202) 586-6074 44. CERAMIC COMPONENTS FOR STATIONARY ORNL Contact: Mike Karnitz, (423) 576-5150 GAS TURBINES IN COGENERATION SERVICE $4,000,000 Gas turbine manufacturers have stated a need for a DOE Contact: Pat Hoffman, (202) 586-6074 turbine inlet temperature of greater than 2600°F in order Solar Contact: Jeff Price, (619) 544-5538 to achieve higher efficiencies. New materials developments are necessary to achieve these temperatures for The performance of stationary gas turbines is limited by extended operating periods. Advanced casting the temperature and strength capabilities of the metallic techniques, metallurgy and coating science will be structural materials in the engine hot section. To realize applied to gas turbines to allow higher operating the benefits of higher temperature, uncooled ceramics temperature for increased efficiency while producing with superior high temperature strength and durability fewer emissions. The goals of these projects are with lower emissions signature will be substituted for improved turbine airfoil castings and reliable, higher metallic parts in the engine hot section. The ceramic performance thermal barrier coatings that will allow for parts comprise the first stage ceramic blades, first stage increased turbine inlet temperature. ceramic nozles and ceramic composite combustor liners. This project will design and test these Keywords: Gas Turbines, Castings, Thermal Barrier components for a stationary 4.0 Mw gas turbine for Coatings cogeneration service. The project will culminate in a 4000-hour field demonstration of the engine. CONTINUOUS FIBER CERAMIC COMPOSITES (CFCC) PROGRAM Keywords: Structural Ceramics, Ceramic Composites, Cogeneration, Gas Turbines The Continuous Fiber Ceramic Composites (CFCC) Program operates as a collaborative effort between MATERIALS PROPERTIES, BEHAVIOR, industry, national laboratories, universities and the CHARACTERIZATION OR TESTING government to develop advanced ceramic composite materials to a point at which the industry will assume 45. LONG-TERM TESTING OF CERAMIC full risk of further development. There are currently six COMPONENTS FOR STATIONARY GAS industrial teams developing more than 20 industrial TURBINES applications for continuous fiber ceramic composite $350,000 materials. The National Laboratories along with DOE Contact: Pat Hoffman, (202) 586-6074 Universities are developing supporting technologies ORNL Contact: Matt Ferber, (423) 576-0818 (e.g. material design, processing methods, manufacturing techniques) and conducting performance Compared to aircraft turbines, the service life evaluations. The DOE program managers are requirements for land-based Advanced Turbine Merrill Smith, (202) 586-3646 and Debbie Haught, Systems (ATS) significantly affect the objectives of (202) 586-2211. respective materials development programs. Land-based turbines generally operate under longer maintenance intervals and endure a high percentage of time under full-load conditions. In addition to cyclic

28 Office of Industrial Technologies

MATERIALS PREPARATION, SYNTHESIS, MATERIALS PREPARATION, SYNTHESIS, DEPOSITION, GROWTH OR FORMING DEPOSITION, GROWTH OR FORMING

47. CFCC PROGRAM - INDUSTRY TASKS 49. INTERMETALLIC ALLOY DEVELOPMENT AND $6,400,000 TECHNOLOGY TRANSFER OF DOE Contact: Merrill Smith, (202) 586-3646 INTERMETALLIC ALLOYS $515,000 The goal of the CFCC Program is to develop, in U.S. DOE Contact: Charles A. Sorrell, (202) 586-1514 industry, the primary processing methods for the ORNL Contacts: M. L. Santella, (423) 574-4805 reliable and cost-effective fabrication of continuous fiber and V. K. Sikka, (423) 574-5112 ceramic composite components for use in industrial applications such as gas turbine components, heat The objective of this project is to develop and apply the exchangers, and hot gas filters. The first phase, excellent oxidation and carburization resistance and completed in 1994, established performance higher strength of intermetallic alloys including nickel requirements of applications and assessed feasibility of aluminides to Industries of the Future-related potential processing systems. Phase two, process manufacturing applications. Progress in bringing engineering and component development, is in technologies to development and commercialization in progress. Industrial participants include Dow Corning, FY 1997 included: (1) research on Ni3AI welding Du Pont Lanxide Composites, Amercom, General technology applicable to, for example, furnace transfer Electric, McDermott Technologies, and Textron. rolls, obtaining materials properties of intermetallic and metallic alloys, modeling of stresses in structural Keywords: Ceramic Composites, Continuous Fiber components, continuation of exposure of furnace fixtures in continuous carburization heat treating MATERIALS PROPERTIES, BEHAVIOR, furnaces (continue to show exceptional corrosion CHARACTERIZATION OR TESTING resistance), (2) evaluating technology for joining thick sections of Ni3AI to dissimilar metals, (3) testing 48. CONTINUOUS FIBER CERAMIC COMPOSITES components in various chemical industry processes, (CFCC) SUPPORTING TECHNOLOGIES (4) completion of the CRADA with GM Saginaw on the $2,000,000 development of Ni3AI for heat treating fixtures, and DOE Contact: Debbie Haught (202) 586-2211 (5) licensed two companies, including Alloy Engineering ORNL Contact: Mike Karnitz, (423) 574-5150 and Casting Company, Sandusky International, to produce Ni3AI materials and components. This project provides basic or generic support to the industry teams conducting CFCC research. Tasks Keywords: Nickel Aluminides, Processing, Steel, include: composite design, materials characterization, Metalcasting, Aluminum, Heat Treating, test methods development, database generation, codes Welding and standards, and life prediction. 50. DEVELOPMENT OF WELDABLE, CORROSION Keywords: Ceramic Composites, Material RESISTANT IRON-ALUMINIDE ALLOYS Characterization, Test Methods $290,000 DOE Contact: Charles A. Sorrell, (202) 586-1514 ADVANCED INDUSTRIAL MATERIALS (AIM) ORNL Contact: P. J. Maziasz, (423) 574-5082 PROGRAM Univ. of Cincinnati Contacts: A. Jordan and O. N. C. Uwakweh (513) 556-3108 New or improved materials can save significant energy and improve productivity by enabling systems to The objectives of this project are to develop FeAI alloys operate at higher temperatures, last longer, and reduce with improved weldability and mechanical and corrosion capital costs. The Advanced Industrial Materials properties for use in structural applications; and to program is a crosscutting program with emphasis on develop the potential for weldable FeAI alloys for use in industrial needs of the Industries of the Future initiative weld-overlay cladding applications. Several develop- and of crosscutting industries including carbon ments were made in FY 1997. New industrial tests of products, forging, heat treating, and welding. Efforts in cast FeAI alloys showed superior oxidation resistance in FY 1996 were focused on partnerships between industry air + 5% water vapor at 1100 C up to 500 h, surprising and the National Laboratories for commercialization of caburization resistance in both oxidizing (H25.5% CH4 - new materials and processes. The program manager is 4.5% CO2 ) and reducing (H2 - 1% CH4) atmospheres, Charles A. Sorrell, (202) 586-1514. and the expected outstanding sulfidation resistance at

29 Office of Industrial Technologies

816°C. Testing of the material in various applications is 52. CONDUCTING POLYMERS: SYNTHESIS AND continuing (neutral salt heat treating baths for steels, INDUSTRIAL APPLICATIONS and molten carbonate salt environments for fuel cells). $250,000 Cast grate bars and pallet tips used in an industrial DOE Contact: Charles A Sorrell, (202) 586-1514 calcination furnace continue to show oxidation/ Los Alamos National Laboratory Contact: sulfidation resistance. Crack-free welds were S. Gottesfeld, (505) 667-0853 successfully made on hot-extrusion (fine grained ingot)- produced FeAI alloys with no pre heat or post heat. For The process of separating pure components out of a the first time, crack free autogenous welds were also mixture of gases is of great industrial importance. made on cast FeAI alloys with pre and post-heat. Current gas separation technologies have major shortcomings, including poor energy efficiency and the Keywords: Iron Aluminides, Coatings, Claddings, generation of secondary pollution. In FY 1997, the use Thermophysical Properties of conducting polymers for electrochemical reactors (ECRS) based on polymeric electrolytes was addressed. 51. COMPOSITES AND COATINGS THROUGH The objective of this effort is to develop and test REACTIVE METAL INFILTRATION electrochemical reactors for the chlor-alkali industry, $443,000 based on polymer membrane/electrode assemblies and DOE Contact: Charles A. Sorrell, (202) 586-1514 on oxygen or air electrodes. In FY 1997, operation of a Sandia National Laboratories Contact: chlor-alkai cell at target cell operating conditions was R. E. Loehman, (505) 844-2222 (includes demonstrated. The system used an oxygen cathode and effort on coating technology at Stanford a commercial chlor-alkali membrane of high current Research Institute) efficiency (>95%).

Ceramic-metal composites have advantages as Keywords: Electrically Conducting Polymers, Gas engineering materials because of their high Separation, Capacitors stiffness-to-weight ratios, good fracture toughness, and because their electrical and thermal properties can be 53. MEMBRANE SYSTEMS FOR EFFICIENT varied through control of their composition and SEPARATION OF LIGHT GASES microstructure. Reactive metal infiltration is a promising $309,000 new route to synthesize and process a wide range of DOE Contact: Charles A. Sorrell, (202) 586-1514 ceramic and metal-matrix composites to near-net-shape Los Alamos National Laboratory Contact: with control of both composition and microstructure. In D. J. Devlin, (505) 667-9914 FY 1997 a detailed mechanistic model was developed for composite formation that explains the observed Ethylene and Propylene are two of the largest microstructure and kinetics as a function of time and commodity chemicals in the U.S. and are major building temperature. This new model has led to a process blocks for other chemicals. More energy-efficient diagram showing the conditions where reactive metal processes are necessary. The main technical objective penetration (RMP) is a practical process. The process of this project is the development and precise control of has also been used to optimize composites of the pore structure of membrane material. Membranes AL2O3-MoSi2, AI203-Mo(Sio93AI,43), and must have specially shaped channels in the 2 to AI203-Mo(Sio.9AI,43)-Mo3AI families, and then 4 nanometer range. In FY 1997, a method for evaluating their properties. developing carbon pores for capillary condensation of hydrocarbons was devised. The use of oblique angle The effort on coating technology at Stanford University sputter techniques to develop thin films with controlled emphasized Al coatings on steel. Coupon specimens pore size has been demonstrated. Separation of butane exhibited excellent corrosion resistance in 1000 hr salt gases form streams containing methane, argon, and spray. hydrogen has been demonstrated. The effort will continue in FY 1998 as a CRADA with Amoco. Keywords: Metal Matrix Composites, Reactive Metal Infiltration, Ceramics, Inorganic Coatings, Keywords: Sputtering, Separations, Olefins, Hydrogen, Corrosion Methane, Membranes

30 Office of Industrial Technologies

54. MICROWAVE AND PLASMA PROCESSING 56. ADVANCED MATERIALS/PROCESSES $275,000 $780,000 DOE Contact: Charles A. Sorrell, (202) 586-1514 DOE Contact: Charles A. Sorrell, (202) 586-1514 Los Alamos National Laboratory Contact: ORNL Contact: P. Angelini, (423) 574-4459, M. Trkula, (505) 667-0591 P. S. Sklad, (423) 574-5069, and C. T Liu, (423) 574-4459 The project focuses on developing coating technologies to obtain erosion, and corrosion resistant, The goals of this project are to develop new and thermodynamically stable, and adherent coatings on die improved materials. Many metallic and ordered materials used to cast aluminum and other metals. Low intermetallic alloys possess unique properties and have temperature organometallic chemical vapor deposition the potential to be developed as new materials for combined with immersion ion processing is being energy related applications. In FY 1997, (1) evaluated developed as the coating technology. In FY 1997, initial the parallelization of a casting program in order to thin film AIN, and amorphous B4C were successfully provide capability for increased throughput and more deposited on steel. Characterization included coating realistic analyses, (2) developed infra-red technology for thickness, composition, mechanical and tribological depositing coatings, surfacing and heating substrate properties. materials, (3) developed initial corrosion resistant Iron-Chromium-Silicon alloys which are applicable in Keywords: Coatings, Chemical Vapor Deposition, Ion various glass industry applications, (4) determined the Processing, Erosion, Corrosion initial weldability of Ni3Si and made significant compositional changes to the alloy. 55. UNIFORM DROPLET PROCESSING $440,000 Keywords: Intermetallics, Ordered Alloys, TiAI, Ni3AI, DOE: Contact: Charles A. Sorrell, (202) 586-1514 Ni3Si, Metalcasting, Glass, Alloys ORNL Contact: Craig A. Blue (423) 574-4351, and Vinod Sikka, (423) 574-5123 MATERIALS PROPERTIES, BEHAVIOR, Massachusetts Institute of Technology Contact: CHARACTERIZATION OR TESTING J-H Chun,(617) 253-1759 Northeastern University Contact: T. Ando, 57. MATERIALS FOR RECOVERY BOILERS (617) 373-3811 $940,000 DOE Contact: Charles A. Sorrell, (202) 586-1514 The purpose of this project is to adapt the uniform ORNL Contact: James R. Keiser, (423) 574-4453 droplet process to higher melting materials e.g., intermetallic alloys, stainless, steel, superalloys; to The purpose of this project is to determine the cause of provide superior metal powders for the powder failure of composite tubes used in Kraft Black Liquor metallurgy industry; and to develop methods for spray recovery boilers during pulp and paper making, and to coating or casting of high temperature materials, develop new materials to eliminate failures. The project including aluminide intermetallics. Spray forming of consists of three efforts: (1) to obtain operating data metallic systems is being investigated. Participants in and failure analyses from pulp and paper companies, the research include Oak Ridge National Laboratory, boiler manufacturers and composite tube Massachusetts Institute of Technology, Northeastern manufacturers, (2) to determine residual stresses in University and powder metal companies. In FY 1997, new and used composite tubes and microstructural (1) a system able to operate at temperatures up to 1500 characteristics of tubes as related to stresses and C was assembled and initial testing begun, (2) failure mechanisms, and (3) to develop new materials additional materials wee produced on the intermediate and/or fabrication methods for improvements in boiler temperature system (1250°C) (including copper and efficiency, service life, and safety. Participants include bronze), and 3) a license of the technology was taken Oak Ridge National Laboratory, Institute of Paper by Uniform Metals Technology for production of copper Science and Technology, and 11 industrial and bronze uniform droplet materials for filter collaborators. In FY 1997: (1) analyses of tube applications in chemical systems. specimens from many mills showed cracks have common characteristics, (2) temperature and strain Keywords: Powder, Near Net Shape Forming, gauges installed in the floor of a recovery boiler indicate Aluminum, Alloys, Steel, Copper, that occasional temperature excursions do occur (10 to Intermetallic Alloys 200°C above normal operating temperature), (3) extended and verified a model showing stress in tubes versus materials properties and boiler operating

31 Office of Industrial Technologies

conditions (developed a response surface indicating that DEVICE OR COMPONENT FABRICATION, alloy 825 and 625 may be more optimum alloys for use BEHAVIOR OR TESTING as cladding), (4) laboratory stress corrosion results (focusing on boiler conditions during start-up or 59. GEL CASTING TECHNOLOGY cool-down) identified various conditions under which $110,000 currently used cladding of 304L would crack, and (5) the DOE Contact: Charles A. Sorrell, (202) 586-1514 research received the Best Paper Award for 1996 from ORNL Contact: M. A. Janney, (423) 576-5183 the Technical Association of the Pulp and Paper Industry (TAPPI). Gelcasting is an advanced powder forming process. It can be used to form ceramic or metal powders into Keywords: Recovery Boilers, Composite Tubes, Pulp simple or complex, near net shapes. The sol-gel and Paper, Alloys, Stresses, Neutron process is being developed in order to produce Residual Stress, Measurements aluminum oxide tubes for use in high-intensity industrial lighting, and H13 steel dies. For the lighting application 58. METALS PROCESSING LABORATORY USER the sol-gel process will produce identical materials at (MPLUS) CENTER lower temperatures and in far less time than do $435,000 (includes $50K from OIT Glass Vision conventional methods which involve prolonged high team) temperature sintering with sintering aids. In FY 1997, DOE Contact: Charles A. Sorrell, (202) 586-1514 the effort relative to the CRADA with OSRAM demon- Oak Ridge National Laboratory Contact: strated: (1) ability to make complex shape optical M. Mackiewicz-Ludtka, (423) 576-4652 and quality AI203, (2) ability to use meltable cores in gel H. W. Hayden, (423) 574-6936 casting to make complex hollow shapes. In additional FY 1997 efforts the ability to machine gel cast metal The Metals Processing Laboratory User (MPLUS) parts was also completed. Technology was developed Center was officially designated as a DOE User Facility to gel cast various metal alloys including, H13, 174ph, in February, 1996. Its primary purpose is to assist U.S. and nickel superalloys. industry and academia in improving energy efficiency and enhancing U.S. competitiveness. MPLUS is Keywords: Gel Casting, Sol Gel, Aluminum Oxide, designed to provide U.S. Industries with access to the Lighting Tubes, H13 Steel, Dies specialized technical expertise and capabilities to solve metals-processing issues that limit the development and 60. MICROWAVE JOINING OF SIC implementation of emerging materials and materials $110,000 processing technologies. MPLUS includes the following DOE Contact: Charles A. Sorrell, (202) 586-1514 primary user centers: Metals Processing, Metal Joining, FM Technologies, Inc. Contact: R. Silberglitt, Metals Characterization and Metals Process Modeling. (703) 425-5111. As of September 30, 1997, a total of 76 MPLUS Proposals were received from 60 companies and The objective of this project is to develop and optimize a universities representing 26 states. Twelve organiza- joining method that can be applied to large scale tions submitted 2 or more proposals for different fabrication of components such as radiant burner tubes projects. Of the 76 proposals, 53 were reviewed, and 31 and high temperature, high pressure heat exchangers. of these 53 User projects were initiated. Ten (10) Microwave joining of both reaction bonded silicon MPLUS projects were completed, and the 23 proposals carbide and sintered silicon carbide has been demon- were either (a) accepted contingent on legal approval, strated for tubes up to 5 cm in diameter. Joints are leak- (b) under development, or c) being modified. A total of tight at service temperature, and have adequate 546 user days were logged during FY 1997. Projects mechanical strength for desired applications. In crosscut all of the seven industries in the Industries of FY 1997 the effort included: (1) joining of continuous the Future initiative; other crosscutting industries fiber-reinforced (CFCC) SiC/SiC composite and sintered including forging, heat treating, and welding; and SiC specimens with SiC formed in situ from pyrolysis of crosscutting programs. either polysiloxane (silicone resin) or allyhydridopoly- carbosilane (AHPCS) precursors, (2) determining the Keywords: Industry, User Center, Metals, Materials, maximum shear strength of joints (microwave Processing, Joining, Properties, processing resulted in joints of comparable strength to Characterization, Modeling, Process those processed conventionally, and (3) joining and

32 Office of Industrial Technologies testing (high temperature strength) 8" long by 1" OD conditions simulating the chemical environment of sintered SiC specimens (under the HiPHES project). interest.

Keywords: Microwave Processing, Microwave Joining, Keywords: High Temperature, Filtration, Chemicals, SiC, Tubes Compatibility

61. SELECTIVE INORGANIC THIN FILMS MATERIALS STRUCTURE AND COMPOSITION $350,000 DOE Contact: Charles A. Sorrell, (202) 586-1514 63. METALLIC AND INTERMETALLIC BONDED Sandia National Laboratories contact: CERAMIC COMPOSITES T. M. Nenoff, (505) 844-0340 $165,000 DOE Contact: Charles A. Sorrell, (202) 586-1514 The purpose of this research is to develop a new class ORNL Contacts: P. F. Becher, (423) 574-5197 and of inorganic membranes for light gas separation and T. N. Tiegs, (423) 574-5173 use this technology to improve separation efficiencies Southern Illinois University: R. Koc, currently available with polymer membranes, (618) 453-7005 particularly for light alkanes. The approach is to nucleate and crystallize zeothlitic phases from sol-gel To improve the reliability of ceramic components, new derived amorphous coatings, using porous filters and approaches to increasing the fracture toughness of gas membranes as supports for these films. In FY1997 ceramics over an extended temperature range are efforts included: (1) initiation of a CRADA with Amoco needed. One method is the incorporation of ductile on the feasibility of using shape selective molecular phases into ceramic matrix alloys for local plastic sieve membranes to enrich p-xylene from mixtures, deformation during crack-bridging processes. This (2) fabrication of cesium phosphate molecular sieve objective of this program is to develop ceramic membranes on porous zinc oxide wafers, (3) production composites with high fracture toughness for of zinc oxide phosphates with larger pores of the intermediate temperature use in wear, tribological and M3Zn(PO4) 3 structure type, and (4) formation of engine applications. In FY 1997 various specimens methylammonium zinc oxide phosphate phase that were tested in a number of environments and a data remains microporous after the water template is information package was prepared. removed. rewrso- otnsPoesnThe effort on ceramic powder processing has the Keywords: Coatings, Sol-Gel Processing objective of developing new synthesis methods using carbothermic reduction of carbon-coated precursors for 62. HIGH TEMPERATURE PARTICLE FILTRATION producing high purity, submicron metal carbide, metal TECHNOLOGY nitride and metal boride systems. During FY1997 efforts $40,000 (project also includes additional effort included: (1) determining carbon content effects of from the CFCC program) resulting TiC composites and the applicability of DOE Contact: Charles A. Sorrell, (202) 586-1514 producing TiB2 powders, (2) preparation of TiC powder, Oak Ridge National Laboratory Contact: - and (3) fabrication of specimens at numerous sites and T. Besmann, (423) 574-6852 subsequent testing of composite specimens.

The objective of this project is to develop high Keywords: Ceramics, Composites, Nickel Aluminide, temperature materials for high temperature filtration Powder needs. High temperature filters are critical in many chemical and other industrial processes. The effort 64. PROCESSING OF POLYMERS IN A MAGNETIC includes bench-scale testing and analyses of FIELD compatibility of materials in various environments. The $341,000 current focus is on filtration technology for the k, DOE Contact: Charles A. Sorrell, (202) 586-1514 dimethyldichlorosilane process. In FY 1997, the CRADA Los Alamos National Laboratory Contacts: with Dow Corning continued. Modification to laboratory M. E. Smith, (505) 665-6858, and furnaces were made for bench scale testing of filter B. C. Benicewicz, (505) 665-0101 specimens. A large number of filter specimens was obtained and each filter was tested for 24 h under The purpose of this project is to demonstrate the utility of magnetic fields, to beneficially modify or control the physical, optical and electrical properties of materials through the application of magnetic fields during

33 Office of Industrial Technologies

polymerization processing and solidification. DEVICE OR COMPONENT FABRICATION, Researchers at Los Alamos National Laboratory, in BEHAVIOR OR TESTING collaboration with an industrial partner, have demonstrated that using high (10-20 Tesla) magnetic 66. HIGH PRESSURE HEAT EXCHANGER SYSTEM fields to orient liquid crystal polymers during processing (HIPHES) ENERGY PRODUCTION can lead to substantial improvements in mechanical $0 properties. In FY 1997, (1) successfully produced DOE Contact: Gideon Varga, (202) 586-0082 polymer composite plaques (approximately 8" x 8" x Solar Turbines Contact: B. Harkins 0.125") of excellent uniformity as determined by visual (619) 544-5398 inspection and mechanical property measurements, (2) demonstrated feasibility of using magnetic fields in The High Pressure Heat Exchanger System (HiPHES) the 1 to 2 Tesla range as provided with commercially uses exhaust heat from a hazardous waste incinerator available magnets, and (3) determined the nature of the to drive a power turbine. Under this concept, a ceramic molecular packing structures as aligned in the magnetic heat exchanger replaces the combustor in the gas field by the use of nuclear magnetic resonance generator section of a combustion turbine. The testing spectroscopy. of a prototype high pressure ceramic heat exchanger for more than 800 hours at 1800°F and 100 psi solved Keywords: Organic Polymers, Magnetic Processing, critical issues of joining, system assembly, and repair. Mechanical Properties This included long term exposure in a dust-laden slip stream of a working hazardous waste incinerator. An COMBUSTION/HEAT EXCHANGER PROGRAM optimal system comprises both monolithic ceramics and ceramic matrix composites. Uncertainties in various The goal of the Combustion Program activities is to market forces for waste incineration has postponed a 4 maximize efficiency and minimize emissions at the Mw demonstration. The technology has been lowest practical cost. The program is designed to move transferred to DOE's Advanced Turbine Systems (ATS) superior combustion concepts for the laboratory through program. industry host site demonstration resulting in commercialization. The DOE program manager is Keywords: Ceramic Composites, Heat Exchangers, Gideon Varga, (202) 586-0082. Waste Incineration

MATERIALS PROPERTIES, BEHAVIOR, 67. HIGH PRESSURE HEAT EXCHANGER SYSTEM CHARACTERIZATION OR TESTING (HiPHES) FOR ETHYLENE PRODUCTION $26,196 65. ADVANCED HEAT EXCHANGER MATERIAL DOE Contact: Gideon Varga, (202) 586-0082 TECHNOLOGY DEVELOPMENT Stone & Webster Engineering Corp. Contact: $630,000 Joe Gondolfe, (281) 368-4379 DOE Contact: G. Varga, (202) 586-0082 ORNL Contact: M. Karnitz, (423) 574-5150 In this project, advanced ceramics are replacing the alloys conventionally used in ethylene production This project conducts research to evaluate advanced reactors. Ethylene production technology is mature, with ceramic materials, fabrication processes and joining technological advances resulting in gains of much less techniques. The effects of hot, corrosive environments than 1 percent. Pilot runs on this project have on candidate ceramic and ceramic composite materials demonstrated a 10 percent increase in ethylene continue to be investigated. Also under investigation is production due to an increase in desirable yield and a the performance of advanced ceramic materials prolonged run time between decoking cycles, achieved subjected to the processing environments encountered under controlled experimental conditions.. in steam cracking for ethylene production. Keywords: Structural Ceramics, Ethylene, Heat Keywords: Structural Ceramics, Corrosion-Gaseous, Exchangers Industrial Waste Heat Recovery, Ethylene

34 Office of Transportation Technologies

OFFICE OF TRANSPORTATION TECHNOLOGIES

FY 1997

Office of Transportation Technologies - Grand Total $24,249,000

Transportation Materials Technoloav $24,249,000

Automotive Materials Technoloyv $17,483,000

Propulsion Systems Materials $5,483,000

Materials Preparation. Synthesis. Deposition. Growth or Forming $3,027,000

Gelcasting: Scale-up and Commercialization 550,000 Optimization of Silicon Nitride Ceramics 177,000 in situ Toughened Silicon Nitride 350,000 Gas Turbine Engine Components Manufacturing Scale-Up and Demonstration 1,200,000 Advanced Automation Gelcasting Processes for Silicon Nitride Components 750,000

Materials Properties. Behavior. Characterization or Testing $1,626,000

Characterization and Life Prediction of Ceramic Recuperator Materials 71,000 Component Verification 275,000 High Frequency Fatigue 250,000 Tensile Stress Rupture Testing 270,000 Toughened Ceramics Life Prediction 200,000 Life Prediction Methodology 0 Environmental Effects in Toughened Ceramics 385,000 Nondestructive Evaluation 175,000

Technoloav Transfer and Management Coordination $ 425,000

Technical Project Management 425,000

Device or Component Fabrication. Behavior or Testing $ 405,000

Corrosion-Resistant Coatings 195,000 Ceramic-Metal Joining 110,000 Mechanical Reliability Assessment of Electronic Ceramics and Electronic Ceramic Components 100,000

Liahtweight Vehicle Materials Technoloqy $12,000,000

Device or Component Fabrication. Behavior or Testing $12,000,000

Low-Cost High Performance Aluminum Alloy Sheet for Automotive Applications 1,250,000 Low-Cost High Performance Cast Light Metals for Automotive Applications 1,300,000 Advanced Materials and Processes for Automotive Applications 375,000 Northwest Alliance for Transportation Technologies (NATT) 2,500,000 Automotive-Related Graduate Fellowships 350,000 Materials and Processes for Propulsion System Applications 650,000 Technology Assessment and Evaluation 450,000 Glass Reinforced Composite Materials Joining, Durability and Enabling Technologies 1,850,000 Composite Material Design, Manufacturing and Demonstration 1,425,000 USAMP Cooperative Agreement 1,000,000 Carbon Fiber Based Composite Materials Technology 850,000

35 Office of Transportation Technologies

OFFICE OF TRANSPORTATION TECHNOLOGIES (continued)

FY 1997

Transportation Materials Technology (continued)

Electric Drive Vehicle Technologies $3,397,000

Advanced Battery Program $2,997,000

Materials Preparation. Synthesis. Deposition. Growth or Forming $ 883,000

Advanced Electrode Research 300,000 Electrochemical Properties of Solid-Electrolytes 200,000 Preparation and Characterization of New Polymer Electrolytes 210,000 New Cathode Materials 73,000 Development of Novel Electrolytes for Rechargeable Lithium Cells 100,000

Materials Properties. Behavior. Characterization or Testing $1,530,000

Carbon Electrochemistry 250,000 Fabrication and Testing of Carbon Electrodes as Lithium Intercalation Anodes 75,000 Reactivity and Safety Aspects of Carbonaceous Anodes in Lithium-Ion Batteries 140,000 Battery Materials: Structure and Characterization 140,000 Polymer Electrolyte for Ambient Temperature Traction Batteries: Molecular Level Modeling for Conductivity Optimization 145,000 Analysis and Simulation of Electrochemical Systems 235,000 Corrosion of Current Collectors in Rechargeable Lithium Batteries 200,000 Electrode Surface Layers 200,000 Microstructural Modeling of Highly Porous NiMH Battery Substrates 145,000

Device or Component Fabrication. Behavior or Testing $ 584,000

Development of a Thin-Film Rechargeable Lithium Battery for Electric Vehicles 71,000 Applied Research on Novel Cell Components for Advanced Capacitors 115,000 Sol-Gel Derived Metal Oxides for Electrochemical Capacitors 123,000 Optimization of Metal Hydride Properties in MH/NiOOH Cells for Electric Vehicle Applications 90,000 Preparation of Improved, Low Cost Metal Hydride Electrodes for Automotive Applications 185,000

Fuel Cell Materials $ 400,000

Materials Properties. Behavior. Characterization or Testing $ 400,000

Electrode Kinetics and Electrocatalysis 300,000 Poisoning of Fuel Cell Electrocatalyst Surfaces: NMR Spectroscopic Studies 100,000

36 Office of Transportation Technologies

OFFICE OF TRANSPORTATION TECHNOLOGIES (continued)

FY 1997

Transportation Materials Technologa (continued)

Heavy Vehicle Materials Technoloav $3,369,000

Materials Preparation. Synthesis. Deposition. Growth or Forming $ 998,000

Cost-Effective SRBSN/Microwave Annealing of Silicon Nitride 400,000 Continuous Sintering of Silicon Nitride Ceramics 148,000 Cost-Effective, High-Toughness Silicon Nitride 350,000 Characterization/Testing of Low CTE Materials 100,000 Low CTE Materials/Diesel Exhaust Insulation 0 Low Cost NZP Powder 0 Advanced Manufacturing of Diesel Engine Turborotors 0 Advanced Manufacturing of Ceramic Exhaust Valves for Diesel Engines 0 Insulating Structural Ceramics for High Efficiency, Low Emission Engines 0 Thick Thermal Barrier Coatings (TTBCs) for Low Emissions, High Efficiency Diesel Engine Components 0 Materials for Low Emissions, High Efficiency Diesel Engine Components 0 Materials for Low Emissions, High Efficiency Diesel Engine Components 0 High Strength Materials for Diesel Engine Fuel Injectors 0

Materials Properties. Behavior. Characterization or Testing $ 770,000

Diesel Exhaust Catalyst Characterization 200,000 Life Prediction Verification 200,000 High Temperature Tensile Testing 250,000 Computed Tomography 120,000 On-Machine Inspection 0 Mechanical Properties of CMZP 0

Technology Transfer and Management Coordination $1,065,000

Technical Project Management 565,000 International Exchange Agreement (IEA) 200,000 Standard Reference Materials 200,000 Mechanical Property Standardization 100,000

Device or Component Fabrication. Behavior or Testing $ 536,000

Thick Thermal Barrier Seal Coatings 33,000 Characterization of Machined Ceramics 200,000 Advanced Machining/Manufacturing 223,000 Next-Generation Grinding Wheel 0 High Speed Grinding 0 Laser-Based NDE Methods 80,000 Grinding Machine Stiffness 0 Next Generation Grinding Spindle 0 Process Cost Model 0 Intelligent Grinding Wheel 0

37 Office of Transportation Technologies

OFFICE OF TRANSPORTATION TECHNOLOGIES

The Office of Transportation Technologies seeks to develop, in cooperation with industry, advanced technologies that will enable the U.S. transportation sector to be energy efficient, shift to alternative fuels and electricity, and minimize the environmental impacts of transportation energy use. Timely availability of new materials and materials manufacturing technologies is critical for the development and engineering of these advanced transportation technologies. Transportation Materials Technologies R&D is conducted by the Office of Advanced Automotive Technologies (OAAT) and the Office of Heavy Vehicle Technologies (OHVT) to address critical needs of automobiles and heavy vehicles, respectively. These activities are closely coordinated between the two offices to ensure non-duplication of efforts. Another important aspect of these activities is the partnership between the federal government laboratories and U.S. industry, which ensures that the R&D is relevant and that federal research dollars are highly leveraged.

Within OAAT, the bulk of the materials R&D is carried out through the Transportation Materials Technologies program, with additional specialty materials R&D in the Electric Drive Vehicle Technologies program. The Transportation Materials Technologies program develops: (a) Automotive Propulsion System Materials to enable advanced propulsion systems for hybrid vehicles, and (b) Lightweight Vehicle Materials to reduce vehicle weight and thereby decrease fuel consumption. The program seeks to develop advanced materials with the required properties and the processes needed to produce them at the costs and volumes needed by the automotive industries. Improved materials for body, chassis, and power train are critical to attaining the challenging performance standards for advanced automotive vehicles. The DOE contacts are Thomas Sebestyen, (202) 586-9727, for automotive propulsion system materials and Joseph Carpenter, (202) 586-1022, for automotive lightweight vehicle materials. The Electric Drive Vehicle Technologies program includes the support of Advanced Battery Materials R&D for electric and hybrid vehicle applications. The DOE contact is Ray Sutula, (202) 586-8064. The program also supports Fuel Cell R&D, which includes materials for proton-exchange membrane (PEM) fuel cells. The DOE contact is JoAnn Milliken, (202) 586-2480.

Within OHVT, the Transportation Materials Technologies program focuses on two areas: (a) Heavy Vehicle Propulsion System Materials, and (b) High Strength Weight Reduction Materials. In collaboration with U.S. industry and universities, efforts in propulsion system materials focus on the materials technology critical to the development of the low emission, 55 percent efficient (LE-55) heavy-duty and multi-purpose Diesel engines, such as: manufacturing of ceramic and metal components for high-efficiency turbocharger and supercharger; thermal insulation, for reducing engine block cooling, lowering ring-liner friction and reducing wear; high-pressure fuel injection materials; and exhaust aftertreatment catalysts and particulate traps. In the area of high strength weight reduction materials, energy savings from commercial trucking is possible with high strength materials which can reduce the vehicle weight within the existing envelope so as to increase payload capacity, and thereby reducing the number of trucks needed on the highways. Increased safety can be obtained by new brake materials and by incorporating highly shock absorbent materials in truck structures for improved control and crashworthiness. The DOE contact is Sidney Diamond, (202) 586-8032.

To support mainly propulsion system materials R&D, the High Temperature Materials Laboratory (HTML) at the Oak Ridge National Laboratory is a modern research facility that houses in its six user centers, a unique collection of instruments for characterizing materials. It supports a wide variety of high-temperature ceramics and metals R&D. The HTML enables scientists and engineers to solve materials problems that limit the efficiency and reliability of advanced energy-conversion systems by providing access to sophisticated state-of-the-art equipment (which few individual companies and institutions can afford to purchase and maintain) and highly trained technical staff. The DOE contact is Sidney Diamond, (202) 586-8032.

38 Office of Transportation Technologies

TRANSPORTATION MATERIALS TECHNOLOGY further improved as well if surface grain growth could be prevented by using proper vapor environment during AUTOMOTIVE MATERIALS TECHNOLOGY annealing.

PROPULSION SYSTEMS MATERIALS Keywords: Physical/Mechanical Properties, Silicon Nitride, Toughened Ceramics MATERIALS PREPARATION, SYNTHESIS, DEPOSITION, GROWTH OR FORMING 70. in situ TOUGHENED SILICON NITRIDE $350,000 68. GELCASTING: SCALE-UP AND DOE Contact: T. M. Sebestyen, (202) 586-9727 COMMERCIALIZATION ORNL Contact: T. N. Tiegs, (423) 574-5173 $550,000 AlliedSignal Ceramic Components Contact: DOE Contact: T. M. Sebestyen, (202) 586-9727 J. M. Wimmer, (310) 512-3183 ORNL Contact: D. P.Stinton, (423) 574-4556 ORNL Contact: S. D. Nunn, (423) 576-1668 The purpose of this effort is to develop an extensive property database for AS800 silicon nitride, to improve The purpose of this work is to develop gelcasting as an its high-temperature properties, and to develop advanced, near-net-shape ceramic forming process advanced fabrication processes for thin-walled capable of manufacturing cost-effective, reliable silicon components. This work is being done to address cost nitride components with industrial partners. The project and property requirements to accelerate the adoption of goals include improving the gelcasting chemical system AS800 into engines, including hybrid electric vehicles. to enhance control of processing parameters and molded part characteristics, and improving gelcasting Keywords: Physical/Mechanical Properties, Silicon compositions and machining methods to produce high- Nitride, Toughened Ceramics precision components with features which are machined in the ceramic body. Surface-preparation techniques 71. GAS TURBINE ENGINE COMPONENTS and mold-release agents which enhance separation of MANUFACTURING SCALE-UP AND, the part from the mold and which yield high-quality DEMONSTRATION surface finish will also be identified. $1,200,000 DOE Contact: T. M. Sebestyen, (202) 586-9727 Keywords: Silicon Nitride, Ceramics, Gelcasting, AlliedSignal Engines Contact: M. L. Easley, Forming (602)231-4242 AlliedSignal Ceramic Components Contact: 69. OPTIMIZATION OF SILICON NITRIDE J. M. Wimmer, (310) 512-3183 CERAMICS Kyocera Industrial Ceramics Contact: $177,000 W. D. Carruthers, (360) 750-6215 DOE Contact: T. M. Sebestyen, (202) 586-9727 ORNL Contact: D. P. Stinton, (423) 574-4556 This project facilitates introduction of monolithic University of Michigan Contact: T. Y. Tien, ceramic components in turbine engines and gathering (313) 764-9449 essential and substantial field experience with these - engines. The objectives are to: (1) improve the The objective of this investigation is to synthesize manufacturing processes for ceramic turbine engine silicon nitride ceramics with optimum flexural strength, components (nozzle vanes and turbine blades/bladed fracture toughness, and creep resistance by using disks) and (2) demonstrate these processes in the statistical experimental designs. The sintering production environment. conditions and the composition of the sintering additives can affect the microstructure of silicon nitride ceramics Keywords: Nozzle Vane, Turbine Blade, Turbine Rotor, and the characteristics of the grain-boundary phase Silicon Nitride, Ceramics, Forming, and, hence, the mechanical properties. It is believed Machining that the mechanical properties of silicon nitride can be optimized by controlling the size and aspect ratio of b- Si3N4 and the nature of the grain-boundary phase. In a related study to optimize the surface finish of silicon nitride materials, the effect of annealing on bend strength of specimens is being investigated. It is believed that the strength of these materials can be

39 Office of Transportation Technologies

72. ADVANCED AUTOMATION GELCASTING 74. COMPONENT VERIFICATION PROCESSES FOR SILICON NITRIDE $275,000 COMPONENTS DOE Contact: T. M. Sebestyen, (202) 586-9727 $750,000 ORNL Contact: D. P. Stinton, (423) 574-4556 DOE Contact: T. M. Sebestyen, (202) 586-9727 ORNL Contact: P. F. Becher, (423) 574-5157 ONR Contact: S. G. Fishman, (703) 696-0285 AlliedSignal Ceramic Components Contact: The objectives of this effort are to: (1) develop test D. D. Foley, (310) 512-5916 methodology to measure mechanical properties of ceramics from complex-shaped components (e.g., gas This project is Enhancement #2 of a DARPA/ONR turbine blades, nozzles, and rotors) at elevated Advanced Materials Partnership Program with the temperatures; and (2) generate a mechanical properties Advanced Structural Ceramics Virtual Company database for recuperator thin sheet ceramic composites (Cooperative Agreement #N00014-95-2-0006). The being developed by Du Pont Lanxide Composites objectives of Enhancement #2 are to: (1) custom design (DLC). The database will be used for the finite element and build equipment system capable of automating the analysis and life prediction of the recuperator gelcasting process, (2) demonstrate capability to components. produce 500 to 1000 turbine wheels per month for a period of two months and (3) integrate the equipment Keywords: Components, Property Characterization, onto the production floor. Silicon Nitride, Toughened Ceramics

Keywords: Silicon Nitride, Ceramics, Gelcasting, 75. HIGH FREQUENCY FATIGUE Forming, Automation $250,000 DOE Contact: T. M. Sebestyen, (202) 586-9727 MATERIALS PROPERTIES, BEHAVIOR, ORNL Contact: D. P. Stinton, (423) 574-4556 CHARACTERIZATION OR TESTING ORNL Contact: K. C. Liu, (423) 574-5116

73. CHARACTERIZATION AND LIFE PREDICTION The objective of this task is to develop the baseline OF CERAMIC RECUPERATOR MATERIALS information on tensile and cyclic fatigue behavior of $71,000 structural ceramics at room and elevated temperatures DOE Contact: T M. Sebestyen, (202) 586-9727 and at frequencies up to 4 kHz. Material behavior ORNL Contact: M. K. Ferber, (423) 576-0818 models for design and life evaluation analysis of Contact: S. F. Duffy, (330) 678-7328 ceramic components are being developed. A benefit of this task will be a baseline database of candidate The purpose of this effort is to characterize the ceramic materials for use by ceramic materials thermomechanical response, define and help establish manufacturers and ceramic components designers, (in conjunction with researchers at ORNL and design fabricators, and users. engineers at Teledyne Ryan) the requisite material database, as well as perform life-prediction estimates Keywords: Cyclic Fatigue, High Temperature for Teledyne Ryans' ceramic recuperator. This effort Properties, Toughened Ceramics, Silicon supports the Hybrid Electric Vehicle (HEV) Program. Nitride, Time-Dependent

Keywords: Components, Design Codes, Life 76. TENSILE STRESS RUPTURE TESTING Prediction, Statistics, Weibull, Fracture, $270,000 Structural Ceramics, Mechanical DOE Contact: T. M. Sebestyen, (202) 586-9727 Properties ORNL Contact: D. P. Stinton, (423) 574-4556 ORNL Contact: K. C. Liu, (423) 574-5116

The objective of this task is to develop the baseline information on tensile stress rupture and time- dependent creep behavior of structural ceramics at

40 Office of Transportation Technologies elevated temperatures. Another goal is to develop 79. ENVIRONMENTAL EFFECTS IN TOUGHENED material behavior models to facilitate design analysis of CERAMICS high-temperature structural components and improve $385,000 their reliability. DOE Contact: T. M. Sebestyen, (202) 586-9727 ORNL Contact: M. K. Ferber, (423) 576-0818 Keywords: High Temperature Properties, Silicon University of Dayton Contact: N. L. Hecht, Nitride, Tensile Testing, Time-Dependent, (513) 229-4341 Toughened Ceramics The objectives of this task are to evaluate high- 77. TOUGHENED CERAMICS LIFE PREDICTION temperature fatigue behavior, develop life-prediction $200,000 analysis, and measure the thermal-mechanical DOE Contact: T. M. Sebestyen, (202) 586-9727 properties of as-sintered versus machined specimens of ORNL Contact: D. P. Stinton, (423) 574-4556 the latest-vintage Si3N4 ceramics. Additional goals NASA - Lewis Research Center Contact: include a better understanding of the degradation J. A. Salem, (216) 433-3313 mechanisms affecting heat engine materials and extension of the database for these candidate ceramic The objective of this research is to develop and verify materials. A final objective is a better understanding of models and test methods for life prediction of brittle the effects of different machining methods on the materials such as in situ toughened ceramics, glasses, mechanical behavior of these candidate ceramics. and intermetallics. A reliability model for anisotropic Currently, the latest-vintage AS-800, SN-281 and brittle materials such as single-crystal intermetallics and SN-282 materials are being evaluated. semiconductors has been developed and will be verified. Keywords: Environmental Effects, Fatigue, Structural Ceramics, Tensile Testing, Time- Keywords: Creep, Fracture Toughness, High Dependent Temperature Properties, Life Prediction, Silicon Nitride, Time-Dependent, 80. NONDESTRUCTIVE EVALUATION Toughened Ceramics $175,000 DOE Contact: T. M. Sebestyen, (202) 586-9727 78. LIFE PREDICTION METHODOLOGY ORNL Contact: D. P. Stinton, (423) 574-4556 $0 ORNL Contact: W. A. Simpson, Jr., DOE Contact: T. M. Sebestyen, (202) 586-9727 (423) 574-4421 ORNL Contact: C. R. Brinkman, (423) 574-5106 The objective of this program is to develop non- AlliedSignal Engines Contact: N. Menon, destructive evaluation techniques capable of detecting (602) 231-1230 critical flaws in structural ceramic components. Acoustic nonlinearity is being used to monitor the initial The objective of this effort is to develop methodologies microstructural state of structural ceramics and to required to adequately predict the useful life of ceramic assess changes in that state as a function of in-service components in advanced heat engines. The Erica and degradation. This approach appears sensitive to Ceramic computer codes are being updated and verified changes occurring at the lattice level (dislocations, via extensive mechanical property characterization, at vacancies, microcracking, etc.) and may provide a ambient and high temperatures, of uni-and-multiaxial means of detecting early-stage (i.e., incipient) test specimens of AS800 silicon nitride. degradation. In addition, advanced techniques are being developed to detect and characterize critical flaws of Keywords: Creep, Failure Analysis, Failure Testing, particular interest to the ceramic community, i.e. Life Prediction, Nondestructive Evaluation, surface and near-surface flaws. Silicon Nitride, Time-Dependent Keywords: NDE, Structural Ceramics, Ultrasonics

41 Office of Transportation Technologies

TECHNOLOGY TRANSFER AND MANAGEMENT 84. MECHANICAL RELIABILITY ASSESSMENT OF COORDINATION ELECTRONIC CERAMICS AND ELECTRONIC CERAMIC COMPONENTS 81. TECHNICAL PROJECT MANAGEMENT $100,000 $425,000 DOE Contact: T. M. Sebestyen, (202) 586-9727 DOE Contact: T. M. Sebestyen, (202) 586-9727 ORNL Contact: D.P. Stinton, (423) 574-4556 ORNL Contact: D. P. Stinton, (423) 574-4556 ORNL Contact: A. A. Wereszczak, (423) 574-7601 The objective of this effort is to help assess the materials and manufacturing technology needs for The objectives of this task are to provide expertise and advanced automotive propulsion systems, formulate characterization facilities for the assessment and technical plans to meet these needs, and prioritize and prediction of mechanical reliability of electronic implement a long-range research and development ceramics (ECs) and electronic ceramic components program. (ECCs), and to utilize life-prediction algorithms to increase service reliability of ECs and ECCs. Keywords: Advanced Heat Engines, Coordination, Management, Structural Ceramics Keywords: Components, Electronics, Failure Analysis, Failure Testing, Life Prediction, Mechanical DEVICE OR COMPONENT FABRICATION, Properties, Reliability BEHAVIOR OR TESTING LIGHTWEIGHT VEHICLE MATERIALS 82. CORROSION-RESISTANT COATINGS TECHNOLOGY $195,000 DOE Contact: T. M. Sebestyen, (202) 586-9727 DEVICE OR COMPONENT FABRICATION, ORNL Contact: D. P. Stinton, (423) 574-4556 BEHAVIOR OR TESTING ORNL Contact: J. A. Haynes, (423) 576-2894 85. LOW-COST HIGH PERFORMANCE ALUMINUM The objectives of this research program are to develop ALLOY SHEET FOR AUTOMOTIVE a coating system to increase the durability of Si3N4 and APPLICATIONS SiC ceramic materials in hostile combustion $1,250,000 environments and to assess coating manufacturability DOE Contact: Joseph Carpenter, (202) 586-1022 which will lead to component demonstration and ORNL Contact: Phil Sklad, (423) 574-5069 commercialization. Laboratory Partners: ORNL, LANL, INEEL, PNNL Industry Partners: Reynolds Metals Company, Keywords: Coatings, Chemical Vapor Deposition, American Society of Mechanical Engineers CVD, Engines, Silicon Nitride, Structural (ASME), Commonwealth Aluminum, ARCO Ceramics, Corrosion Resistance, Mullite Aluminum, Ravenswood Aluminum

83. CERAMIC-METAL JOINING The objectives of this effort are: to develop and $110,000 implement low-cost continuous casting technologies for DOE Contact: T. M. Sebestyen, (202) 586-9727 production of high-quality aluminum sheet; to develop a ORNL Contact: D.P. Stinton, (423) 574-4556 non-heat treatable aluminum alloy sheet product for ORNL Contact: M. L. Santella, (423) 574-4805 automotive applications, such as exterior body panels or structural components; and todemonstrate advanced The objective of this task is to develop a technology for aluminum alloys and forming process for the producing strong, reliable joints between two ceramic manufacture of sheet aluminum components. subassemblies and between a ceramic and a metallic subassembly. Experiments are being done to identify Keywords: Aluminum, Sheet Forming, Extrusion, and understand the effects of chemical reactions that Automotive occur during active metal brazing on the mechanical properties of silicon nitride.

Keywords: Brazing, Joining/Welding, Metals, Structural Ceramics, Silicon Nitride

42 - Office of Transportation Technologies

86. LOW-COST HIGH PERFORMANCE CAST 88. NORTHWEST ALLIANCE FOR LIGHT METALS FOR AUTOMOTIVE TRANSPORTATION TECHNOLOGIES (NATT) APPLICATIONS $2,500,000 $1,300,000 DOE Contact: Joseph Carpenter, (202) 586-1022 DOE Contact: Joseph Carpenter, (202) 586-1022 PNNL Contact: Gary McVay, (509) 375-3762 ORNL Contact: Phil Sklad, (423) 574-5069 Laboratory Partners: PNNL, Albany Research Laboratory Partners: LLNL, ORNL, SNL, INEEL, Center PNNL, ANL Industry Partners: Alcoa, Reynolds, MC-21 Industry Partners: USAMP (Ford, GM, Chrysler), LEP (Ford, GM, Chrysler) NATT is a PNNL initiative comprised of multiple regional industrial sectors brought together to improve The objectives of this effort are: to optimize design U.S. industrial technologies. The principal focus is the knowledge and improve product capability for light- development of technologies to achieve the 50 percent weight, high-strength, cast structural components; to weight reduction required to meet PNGV's objectives. develop a low-cost method for producing prototype tools NATT partners will use their resources to design new for lightweight metals in metal mold processes such as lightweight metals shaping and connecting, and to lower die casting, injection molding, and stamping; to reduce material costs. Some specific objectives of this effort the lead time for production of prototype tools; and to are: to lower the cost of titanium and demonstrate the improve the energy efficiency and cost effectiveness of feasibility of manufacturing a cost-competitive/ large-scale automotive aluminum die castings by performance enhanced product; to develop an extending die life and reducing die wear. alternative molten salt electrolyte to be used in the low- cost electrowinning of primary magnesium metal; to Keywords: Aluminum, Magnesium, Cast Metals, develop and optimize tailored aluminum blank fabrica- Rapid Prototyping, Automotive, Die Life, tion and forming characteristics for high-volume, low- Die Wear, Die Castings cost automotive panels and structures; to develop a new low-cost process for the efficient on-site stir-casting 87. ADVANCED MATERIALS AND PROCESSES of aluminum metal matrix composites suitable for the FOR AUTOMOTIVE APPLICATIONS production of automotive components and an efficient $375,000 and economical machining process for finishing Al- DOE Contact: Joseph Carpenter, (202) 586-1022 MMC castings; and to develop efficient, cost competitive ORNL Contact: Phil Sklad, (423) 574-5069 technologies for sorting shredded aluminum automotive Laboratory Partners: Ames Laboratory, ORNL scrap. University Partners: University of Wisconsin- Milwaukee Keywords: Titanium, Aluminum, Magnesium, Tailor Industry Partners: USAMP (Ford, GM, Welded Blanks, Scrap Sorting, Metal Matrix Chrysler), The Electric Power Research Composite Institute (EPRI) 89. AUTOMOTIVE-RELATED GRADUATE The objectives of this effort are: to develop low cost FELLOWSHIPS powder metallurgy (PM) manufacturing methods for $350,000 particle reinforced aluminum (PRA) composite DOE Contact: Joseph Carpenter, (202) 586-1022 components; to advance PRA machining technology ORNL Contact: Arvid Pasto, (423) 574-5123 and PRA composite design methodologies; and to produce and evaluate the use of aluminum The fellowship program, administered by the High 'ashalloys'-metal matrix composites that incorporate Temperature Materials Laboratory (HTML) of Oak Ridge coal fly ash-in the commercial manufacture of cast National Laboratory through Oak Ridge Associated automotive parts. Universities (ORAU), sponsors Master's and Ph.D degree students who are U.S. citizens and are Keywords: Metal Matrix Composites, Powder interested in pursuing a career in the area of lightweight Metallurgy, Aluminum, Particle Reinforced materials for automotive applications. Projects must be Aluminum relevant to interest areas of the Office of Advanced Automotive Technologies (OAAT). The objectives of the program are to provide a mechanism for training researchers in state-of-the-art advanced

43 Office of Transportation Technologies characterization techniques using instruments at HTML 92. GLASS REINFORCED COMPOSITE MATERIALS and encourage research in areas of interest to OAAT JOINING, DURABILITY AND ENABLING and DOE. TECHNOLOGIES $1,850,000 Keywords: Graduate Fellowship, Lightweight DOE Contact: Joseph Carpenter, (202) 586-1022 Materials, Automotive Applications, ORNL Contact: Dave Warren (423)574-9693 Characterization Technique Laboratory Partners: ORNL, LBNL Industry and University Partners: USAMP/ 90. MATERIALS AND PROCESSES FOR Automotive Composites Consortium, University PROPULSION SYSTEM APPLICATIONS of Texas, University of Tennessee, Oak Ridge $650,000 Institute of Science and Technology, Tennessee DOE Contact: Joseph Carpenter, (202) 586-1022 State University, Goodrich, Baydur Adhesives, ORNL Contact: Phil Sklad, (423) 574-5069 University of Tulsa Laboratory Partners: ORNL, SNL, LBNL Industry Partners: USAMP (Ford, GM, and The objective of this effort is to develop critical enabling Chrysler), National Center for Machining technologies necessary for the implementation of Sciences advanced structural composite materials. These nclude long term durability test methodologies, durability-driven The objective of these efforts are: to develop a multi- design guidelines, adhesive test methods, non- physics computational model of the induction heating destructive inspection techniques and material models and hardening process in order to predict part which can be used in designing automotive compo- performance; to develop science-based, closed-loop nents. Specific technology thrust areas include the controllers applicable to a broad range of steels; to use development of Mode I, Mode II, and Mixed Mode these tools to develop steel components with optimized, Fracture test methods and computer-based models for strength-to-weight ratios; to develop a model and adhesively bonded joints. This work includes the methodology, based on finite element techniques, that characterization of bulk adhesives, sheet composite, predicts changes in the size and shape of parts that are and adhesive-adherend pairs using three composite attributable to heat treatment (heat treat distortion), and adherends and three adhesives (2 epoxy and 1 thus to provide the ability to optimize designs before urethane). Models are to simulate the fracture behavior heat treatment; and to increase the quality of wear- of bonded joints under a wide range of mode mixes and coated engine blocks by using nondestructive define the fracture envelope. Composite research is to evaluation techniques. lead to the development of experimentally-based, durability-driven design guidelines to assure the long- Keywords: Induction Hardening, Heat Treat Distortion, term (15 year) integrity of polymeric composite Nondestructive Evaluation, Steel automotive structures. The project will develop and demonstrate reliable attachment technologies for use in 91. TECHNOLOGY ASSESSMENT AND lightweight composite structures for automotive EVALUATION applications. Adhesive joint and composite research $450,000 includes bulk material characterization, fracture, fatigue, DOE Contact: Joseph Carpenter, (202) 586-1022 creep, and creep fracture. This work also includes the ORNL Contact: Phil Sklad, (423) 574-5069; development of NDE methods, advanced curing Dave Warren, (423)574-9693, Dick Ziegler, technologies and structural analysis models. (423) 574-5149 Technology implementation is conducted through Laboratory Partners: ORNL Automotive Composites Consortium (ACC) focal projects. An additional objective is to develop NDE The objective of these activities is: to provide technology to evaluate bonded joint integrity of assessment of the cost effectiveness of various automotive assemblies, such as a body-in-white. technologies; to evaluate the ability of the industrial infrastructure to accommodate emerging technologies; Keywords: Polymer, Composites, Joining, Fracture, and to provide guidance to program management as to Durability, Automotive, Adhesives, Non- appropriate investments for R&D funding. Destructive Inspection

Keywords: Cost, Infrastructure

44 Office of Transportation Technologies

93. COMPOSITE MATERIAL DESIGN, automotive suppliers, universities, and private research MANUFACTURING AND DEMONSTRATION institutions. $1,425,000 DOE Contact: Joseph Carpenter, (202) 586-1022 Keywords: Polymer Composites, Aluminum, ORNL Contact: Dave Warren, (423) 574-9693 Magnesium, Free Machining Steel, Glass Laboratory Partners: ORNL, LLNL, INEEL Fiber Preforming, Adhesive Bonding, Slurry Industry and University Partners: USAMPI Preforming, Powder Metallurgy, MMC, Automotive Composites Consortium, Rapid Prototyping, NDT, Automotive University of Michigan, University of Santa Barbara, University of Cincinnati, Wayne State 95. CARBON FIBER BASED COMPOSITE University, Stanford University, University of MATERIALS TECHNOLOGY Nottingham, Michigan Materials and $850,000 Processing Institute, Budd Company, Dow DOE Contact: Joseph Carpenter, (202) 586-1022 ORNL Contact: Dave Warren, (423) 574-9693 The objective is to develop the design and manu- Laboratory Partners: ORNL facturing methodologies to allow safe, reliable, Industry Partners: USAMP/Automotive Composites repeatable and cost- effective implementation of Consortium, Lambda Technologies, AKZO composite materials in automotive structures. Specific Fortafil Fibers, Amoco efforts include the following: develop and model slurry preforming processes applicable to the automotive The objective is to conduct materials research to lead to industry. After initial development, optimize the the development of low cost carbon fiber for automotive processes for repeatabilty of glass fiber positioning at applications. Research includes investigation of increased production rates. In cooperation with the ACC alternate energy deposition methods, and alternate Energy Management working group, develop material precursors for producing carbon fiber, as well as the and component models for composite materials in high development of improved thermal processing methods energy impacts for prediction of passenger safety and and equipment for fiber manufacture. This work optimization of component designs. Demonstrate key examines the fiber architecture and manufacturing technologies through focal projects which incorporate issues associated with carbon fiber usage to take advances from various projects into manufacturable, advantage of this material's hiqh strength and modulus, cost effective pre-production prototypes that meet or while minimizing the effects of its low strain to failure. exceed the requirements of current production Candidate resin systems are screened for potential of assemblies. meeting automotive industry requirements.

Keywords: Polymer, Composites, Crash, Energy Keywords: Polymer, Composites, Carbon Fiber Management, Processing, Automotive, Preforming, Molding ELECTRIC DRIVE VEHICLE TECHNOLOGY

94. USAMP COOPERATIVE AGREEMENT ADVANCED BATTERY PROGRAM $1,000,000 DOE Contact: Joseph Carpenter, (202) 586-1022 MATERIALS PREPARATION, SYNTHESIS, ORO Contact: Harold Clark, (423) 576-0823 DEPOSITION, GROWTH OR FORMING Industry Partner: US Automotive Materials Partnership (Chrysler, Ford, GM), Aplicator, 96. ADVANCED ELECTRODE RESEARCH Budd $300,000 DOE Contact: Ray Sutula, (202) 586-8064 The objectives of this project are to define and conduct Lawrence Berkeley National Laboratory vehicle-related R&D in materials and materials Contact: E. J. Cairns, (510) 486-5028 processing. Projects include Rapid Prototyping for Metal Mold Processes, Design and Product Optimization for The objective of this project is to investigate the Cast Light Metals, Powder Metallurgy of Particle behavior of S electrodes in Li/polymer electrolyte/ sulfur Reinforced Aluminum, Non-Toxic Free Machining Steel, cells and improve their lifetime and performance. Slurry Process Scale-up, P4 Preforming, Full Field NDT Interest in the Li/S couple stems from its high of Adhesive Bonding, ACC Focal Project II and ACC theoretical specific energy (-2600 Wh/kg) as well as its Focal Project ll. Projects will be conducted by multi- environmentally benign components. In principle, this organizational teams involving USAMP members, system is well-suited to EV applications, however a practical Li/S battery showing promise for EVs has not

45 Office of Transportation Technologies

been developed. By using lower-density acetylene which are useful as positive electrodes in advanced black, greatly improved utilization of the sulfur active nonaqueous rechargeable batteries. Cycling studies on material in the range of 40% and higher was LixMyMnO 2 (M = Li, Na, K) showed that the highest demonstrated. capacity and longest life was obtained when M = K, which provided the largest interlayer spacing. Keywords: Batteries, Solid-State Cells, Electric Vehicles, Sulfur Electrode Keywords: Intercalation Electrodes, Rechargeable Batteries 97. ELECTROCHEMICAL PROPERTIES OF SOLID- ELECTROLYTES 100. DEVELOPMENT OF NOVEL ELECTROLYTES $200,000 FOR RECHARGEABLE LITHIUM CELLS DOE Contact: Ray Sutula, (202) 586-8064 $100,000 Lawrence Berkeley National Laboratory DOE Contact: Ray Sutula, (202) 586-8064 Contact: L. C. De Jonghe, (510) 486-6138 Delaware State University Contact: K. Wheeler, (302) 739-4934 The objective of this project is to fabricate and study novel composite electrolytes which combine the The objective of this project is to investigate alternative advantages of a protective thin-film single-ion conductor electrolytes for rechargeable lithium batteries. Families with a conventional elastomeric polymer electrolyte for of chloroaluminate-based ionic liquids were considered. EV applications. A study of the transport properties of Electrochemical studies revealed that electrolytes PEO-NaTFSI (TFSI=N(CF3SO) 2 ) electrolytes was containing imidazole and AICI 3 had a relatively large completed, and thin solid films of Li3Lao.7.TiO3 were electrochemical window of 4 V. prepared by hydraulically pressing powders under an inert atmosphere. Keywords: Intercalation Electrodes, Rechargeable Batteries Keywords: Batteries, Solid-State Cells, Electric Vehicles, Polymeric Electrolytes MATERIALS PROPERTIES, BEHAVIOR, CHARACTERIZATION OR TESTING 98. PREPARATION AND CHARACTERIZATION OF NEW POLYMER ELECTROLYTES 101. CARBON ELECTROCHEMISTRY $210,000 $250,000 DOE Contact: Ray Sutula, (202) 586-8064 DOE Contact: Ray Sutula, (202) 586-8064 Lawrence Berkeley National Laboratory Lawrence Berkeley National Laboratory Contact: J. Kerr, (510) 486-6279 Contact: K. Kinoshita, (510) 486-7389

The objectives of this project are to develop methods of The objective of this project is to identify the critical preparation and purification of the comb-branch parameters that control the reversible intercalation of Li backbone structures to design new polymers for rapid in carbonaceous materials and to determine their ion transport in batteries and to measure lithium ion maximum capacity for Li intercalation. The collaboration transference numbers as a function of polymer and Li with Superior Graphite and LLNL continued with the salt structure. Polymer electrolytes containing focus to evaluate alternative graphitized carbons for the oxymethylene-linked polyethylene glycol and negative electrodes in Li-ion cells. The graphitized polypropylene oxide were prepared. carbons obtained from Superior Graphite so far have demonstrated that high heat-treatment temperatures Keywords: Batteries, Solid-State Cells, Electric (-2800°C) may not be required to obtain acceptable Vehicles, Polymeric Electrolytes electrode materials for Li-ion cells.

99. NEW CATHODE MATERIALS Keywords: Carbon, Li Batteries, Li intercalation $73,000 DOE Contact: Ray Sutula, (202) 586-8064 State University of New York Contact: M. S. Whittingham, (607) 777-4623

The objective of this project is to synthesize and evaluate oxides of tungsten, molybdenum, and first-row transition metals for alkali-metal intercalation electrodes

46 Office of Transportation Technologies

102. FABRICATION AND TESTING OF CARBON 104. BATTERY MATERIALS: STRUCTURE AND ELECTRODES AS LITHIUM INTERCALATION CHARACTERIZATION ANODES $140,000 $75,000 DOE Contact: Ray Sutula, (202) 586-8064 DOE Contact: Ray Sutula, (202) 586-8064 Brookhaven National Laboratory Contact: Lawrence Livermore National Laboratory J. McBreen, (516) 282-4071 Contact: T Tran, (510) 422-0915 The objective of this research is to elucidate the The objectives of this work are to evaluate the perfor- molecular aspects of materials and electrode processes mance of carbonaceous materials as hosts for lithium in batteries and to use this information to develop intercalation negative electrodes, and to develop electrode and electrolyte structures with good reversible lithium intercalation negative electrodes for performance and long life. Current efforts have included advanced rechargeable lithium batteries. The approach in situ extended x-ray absorption fine structure (EXAFS) is to fabricate electrodes from various commercial studies of lithium manganese oxides and nickel oxide carbons and graphites and evaluate them in small electrodes. The EXAFS study shows that midway lithium-ion cells. Electrode performance will be through the charge there is considerable disorder in the correlated with carbon structure and properties in LiNiO2 material, but it reverts to a more ordered collaboration with LBNL. The Li intercalation capacities structure towards the end of charge. On the other hand, of petroleum needle cokes (190LS, Superior Graphite LiMn 204 shows much less changes in the spinel Co.) that were air milled and heat treated to 1800°, structure during charge than LiNiO2. 2100° or 2350°C were examined The highest Li intercalation capacity (x = 0.93 in LixC6) was obtained Keywords: Electrodes, Batteries, EXAFS with the sample that was heat treated at 2350°C and then air milled. 105. POLYMER ELECTROLYTE FOR AMBIENT TEMPERATURE TRACTION BATTERIES: Keywords: Carbon, Li Batteries, Intercalation MOLECULAR LEVEL MODELING FOR CONDUCTIVITY OPTIMIZATION 103. REACTIVITY AND SAFETY ASPECTS OF $145,000 CARBONACEOUS ANODES IN LITHIUM-ION DOE Contact: Ray Sutula, (202) 586-8064 BATTERIES Northwestern University Contact: M. A. Ratner, $140,000 (708) 491-5371 DOE Contact: Ray Sutula, (202) 586-8064 University of Michigan Contact: Abbas Nazri, The goal of this research is to apply molecular (810) 986-0737 dynamics (MD) and Monte Carlo simulations to understand the conduction process in polymer The objective of this research is to investigate the electrolytes, and its modification by such parameters as chemical, electrochemical and safety aspects of carbon temperature, density, ion species, polymer chain anodes used in Li-ion batteries, and to identify the basicity, and interionic correlations, The results of this reaction products that form during charge discharge study should be beneficial in the development of cycling. This project was a new initiative in FY 1997. improved polymer electrolytes for rechargeable Li Initial results indicate that a large amount of gaseous batteries for EV applications. A simple model was species is generated on graphitic carbons when mixed developed in which the polyelectrolyte species are cyclic carbonate and alkyl carbonate-based electrolytes semibound, i.e. they cannot diffuse long distances. this are used. model suggests that more flexible polyelectrolytes will have smaller diffusion barriers and higher ionic Keywords: Carbon, Li Batteries, Li intercalation, conduction. Electrolyte Decomposition Keywords: Batteries, Electric Vehicles, Polymeric Electrolytes

47 Office of Transportation Technologies

106. ANALYSIS AND SIMULATION OF ellipsometry, light scattering, Raman spectroscopy and ELECTROCHEMICAL SYSTEMS scanning electron microscopy are utilized to monitor the $235,000 formation of surface layers on secondary battery DOE Contact: Ray Sutula, (202) 586-8064 electrodes. Quantitative analysis of the SER spectra of University of California, Berkeley Contact: a Ni/Ni(OH)2 electrode showed that the precursor J. Newman, (510) 642-4063 a-Ni(OH)2 phase is only partially converted into P-Ni(OH)2 during cycling. Cyclic voltammetry of TiO2- The objective of this program is to improve the modified Ni electrode shows that TiO2 addition does not performance of electrochemical cells used in the inter- significantly shift the O2-evolution potential. conversion of electrical energy and chemical energy by identifying the phenomena which control the perfor- Keywords: Ion Implantation, Electrodes, Rechargeable mance of a system. These phenomena are incorporated Batteries into a mathematical model which can predict system behavior. The models aid in the recognition of important 109. MICROSTRUCTURAL MODELING OF HIGHLY parameters that are crucial to the optimization of a POROUS NiMH BATTERY SUBSTRATES given electrochemical system. A mathematical model $145,000 has been developed which showed good agreement DOE Contact: Ray Sutula, (202) 586-8064 with data obtained by slow charge/discharge potential University of Michigan Contact: transients, cyclic voltammetry, and potential-step Ann Marie Sastry, (313) 764-3061 measurements using a nickel hydroxide-hydrogen thin film cell. These data compare well with output from the The objective of this research is to develop predictive numerical model. capability for determining performance of MH/NiOOH secondary cells through microstructural modeling of the Keywords: Electrochemical Phenomena, NiOOH electrode. Galvanostatic Charge/Discharge These studies should lead to improved energy densities 107. CORROSION OF CURRENT COLLECTORS IN in MH/NiOOH batteries by determining optimal micro- RECHARGEABLE LITHIUM BATTERIES structures for NiOOH substrates. The study is focused $200,000 on the effects of the microstructure of fibrous composite DOE Contact: Ray Sutula, (202) 586-8064 electrodes on thermal and electrical conductivity, University of California, Berkeley Contact: strength, and lifetime. Studies on a variety of fibers, J. W. Evans, (510) 642-3807 including carbon (7-12 /um diameter) and polypropylene (-10 /m diameter) fibers, both coated with nickel and The objective of this research is to investigate the sinter-bonded, and pure sinter-bonded nickel fibers, corrosion behavior of current collectors for rechargeable were completed. A novel network generation approach Li batteries. It was observed that, after short-term has been validated with experimental resistivities in normal cycle tests of LiN6O13 cells, only a small amount fibrous substrates, and a new mechanics technique has of corrosion pits appeared on Al collectors, but serious been developed to model the damage progression in the pitting corrosion occurred after overcharging. fibrous substrates, and damage simulations have been initiated. Keywords: Current Collectors, Advanced-Batteries Keywords: MH/NiOOH Batteries Modeling, 108. ELECTRODE SURFACE LAYERS Microstructural Characterization $200,000 DOE Contact: Ray Sutula, (202) 586-8064 Lawrence Berkeley National Laboratory Contact: F. R. McLarnon, (510) 486-4636

Advanced in situ and ex situ characterization techniques are being used to study the structure, composition, and mode of formation of surface layers on electrodes used in rechargeable batteries. The objective of this research is to identify film properties that improve the rechargeability, cycle-life performance, specific power, specific energy, stability, and energy efficiency of electrochemical cells. Sensitive techniques such as

48 Office of Transportation Technologies

DEVICE OR COMPONENT FABRICATION, 112. SOL-GEL DERIVED METAL OXIDES FOR BEHAVIOR OR TESTING ELECTROCHEMICAL CAPACITORS $123,000 110. DEVELOPMENT OF A THIN-FILM DOE Contact: Ray Sutula, (202) 586-8064 RECHARGEABLE LITHIUM BATTERY FOR University of Wisconsin - Madison Contact: ELECTRIC VEHICLES Marc A. Anderson, (608) 262-2674 $71,000 DOE Contact: Ray Sutula, (202) 586-8064 The objective of this research is to improve the Oak Ridge National Laboratory Contact: chemical and materials properties of the NiO/Ni system J. B. Bates, (615) 574-4143 for electrochemical capacitors (ultracapacitors). Proto- types made from nickel oxide thin-film electrodes have The objective of this research is to identify methods for been successfully fabricated with a total thickness of the depositing acceptable thin-film electrodes for cell (including outside packaging material) of less than 1 rechargeable Li batteries. These methods are being mm. Five cells were tested at INEEL; results are applied to develop solid-state Li/LixMn 2O4 rechargeable documented in an INEEL report. This project has been thin-film Li batteries for EV applications. The batteries completed. are expected to have several-important advantages as power sources: high specific energy and energy density, Keywords: Electrochemical Capacitor, NiO Electrodes long cycle lifetimes, and a wide temperature range of operation. Laboratory-scale solid-state cells with 113. OPTIMIZATION OF METAL HYDRIDE LiMn2O4 electrodes were fabricated with open circuit PROPERTIES IN MH/NiOOH CELLS FOR voltages (OCVs) between 2.98 and 4.03 V, consistent ELECTRIC VEHICLE APPLICATIONS with the cathode composition with x = 1 for LixMn 2O4. $90,000 Studies indicate that the cathode surface has undergone DOE Contact: Ray Sutula, (202) 586-8064 a phase change to the orthorhombic structure for x > 1, University of South Carolina Contact: and the cell resistance increased as a result of the initial .R. E. White, (803) 777-7314 discharge. The objective of this research is to optimize the alloy Keywords: Electric Vehicles, Thin-Film Batteries, composition of metal hydride electrodes by micro- Solid-State Electrodes encapsulation of hydrogen storage alloys metal hydride electrodes for MH/NiOOH batteries. Microencapsulation 111. APPLIED RESEARCH ON NOVEL CELL of the hydrogen storage alloys with electroless nickel or COMPONENTS FOR ADVANCED CAPACITORS cobalt-nickel coatings was found to improve the cycle $115,000 life by forming a conductive passive film on the surface DOE Contact: Ray Sutula, (202) 586-8064 which prevents the oxidation of the active materials. SAFT Research & Development Center Contact: Guy Chagnon, (410) 771-3200 Keywords: MH/NiOOH Batteries, Hydrogen Storage, LaNi427Sno24 Alloy, Microencapsulation The objective of this research is to evaluate the double- layer capacitance of high-surface-area carbons, and to 114. PREPARATION OF IMPROVED, LOW COST develop low-cost carbon electrodes for electrochemical METAL HYDRIDE ELECTRODES FOR double-layer capacitors that meet the DOE goal of AUTOMOTIVE APPLICATIONS 1600 W/kg, 10 Wh/kg and $1/kW. Cells with 140°F $185,000 capacitance and 20 milliohms resistance, corresponding DOE Contact: Ray Sutula, (202) 586-8064 to high-performance capacitors delivering 6.1 Wh/kg Brookhaven National Laboratory Contact: and 3.9 Kw/kg were built and tested. An additional J. Reilly, (516) 344-4502 10 cells were fabricated and tested at INEEL; results (typically 1.4-1.8 Wh/kg at about 63 W/kg) are The objective of this research is to increase the energy documented in an INEEL report. This project has been density of metal hydride electrodes for MH/NiOOH completed. batteries by preparing improved AB5 and AB2 electrodes. A second objective is to develop improved Keywords: Electrochemical Capacitors, Carbon mathematical model for the electrochemical behavior of Electrodes the MHx electrode. The presence of cobalt and Al in AB5 hydride electrodes was found to strongly inhibit corrosion by reducing the lattice expansion and contraction in the electrochemical charge-discharge

49 Office of Transportation Technologies process and, in the case of Co, from the formation of a electrooxidation on Pt-based electrocatalysts by NMR. corrosion-resistant surface layer. The unwanted coupling of the NMR sample to the coil was eliminated, thereby permitting the acquisition of Keywords: MH/NiOOH Batteries Ab5 and Ab2 meaningful NMR spectra of fuel-cell electrode surface Electrodes, Hydrogen Storage, X-ray species under open-circuit conditions and strongly Absorption Spectroscopy suggesting the possibility of acquiring spectra under conditions of in situ electrode potential control. FUEL CELL MATERIALS Keywords: NMR, Electrooxidation, Fuel Cells MATERIALS PROPERTIES, BEHAVIOR, CHARACTERIZATION OR TESTING HEAVY VEHICLE MATERIALS TECHNOLOGY

115. ELECTRODE KINETICS AND MATERIALS PREPARATION, SYNTHESIS, ELECTROCATALYSIS DEPOSITION, GROWTH OR FORMING $300,000 DOE Contact: JoAnn Milliken, (202) 586-2480 117. COST-EFFECTIVE SRBSNIMICROWAVE Lawrence Berkeley National Laboratory ANNEALING OF SILICON NITRIDE Contact: P. N. Ross, (510) 486-6226 $400,000 DOE Contact: Sidney Diamond, (202) 586-8032 Physically meaningful mechanistic models are essential ORNL Contact: D. R. Johnson, (423) 576-6832 for the interpretation of electrode behavior and are ORNL Contact: J. O. Kiggans, (423) 574-8863 useful in directing the research on new classes of materials for electrochemical energy conversion and There are two major objectives of this research element. storage devices. The objective of this project is to The first objective is the development of new sintered develop an atomic-level understanding of the processes reaction-bonded silicon nitride (SRBSN) materials that taking place in complex electrochemical reactions at will serve as cost-effective materials for use in suitable electrode surfaces. Researchers are employing low heavy-duty-diesel applications. The second is the energy electron diffraction (LEED) to study single investigation of microwave heating as a means for the crystals; high resolution electron microscopy (HREM) nitridation of silicon for the fabrication of sintered for carbon electrode materials; and X-ray absorption reaction-bonded silicon nitride. fine structure (EXAFS) for organometallic catalysts. Low Energy Ion Scattering (LEIS) and Auger Electron Keywords: Annealing, Cost-Effective Ceramics, Spectroscopy (AES) are being utilized to study the Microwave Processing, Microwave composition of sputtered and UHV-annealed Sintering, Silicon Nitride, SRBSN polycrystalline Pt-based bulk alloys for hydrogen electrocatalysis. It was found that both the surface and 118. CONTINUOUS SINTERING OF SILICON bulk composition of Pt75Mo25 alloy for hydrogen NITRIDE CERAMICS oxidation was the same. $148,000 DOE Contact: Sidney Diamond, (202) 586-8032 Keywords: Spectrographic Analysis, Electrocatalysts, ORNL Contact: T. N. Tiegs, (423) 574-5173 Electrooxidation Southern Illinois University Contact: D. E. Wittmer, (618) 453-7006/7924 116. POISONING OF FUEL CELL ELECTROCATALYST SURFACES: NMR The objective of this effort is to investigate the potential SPECTROSCOPIC STUDIES of cost-effective sintering of Si3N4 through the $100,000 .development of continuous sintering techniques and the DOE Contact: JoAnn Milliken, (202) 586-2480 use of lower cost Si3N4 powders and sintering aids. Lawrence Berkeley National Laboratory Contact: E. J. Cairns, (510) 486-5028 Keywords: Cost-Effective Ceramics, Silicon Nitride, Sintering Platinum-is the most active single-component catalyst for CH30H electrooxidation in DMFCs; however, poisoning reactions at the surface render the anode ineffective under target operation conditions. The objective of this research is to obtain information on the nature of the poisoning intermediate(s) in CH3OH

50 Office of Transportation Technologies

119. COST-EFFECTIVE, HIGH-TOUGHNESS 121. LOW CTE MATERIALSIDIESEL EXHAUST SILICON NITRIDE INSULATION $350,000 $0 DOE Contact: Sidney Diamond, (202) 586-8032 DOE Contact: Sidney Diamond, (202) 586-8032 ORNL Contact: D. R. Johnson, (423) 576-6832 ORNL Contact: D.R. Johnson, (423) 576-6832 ORNL Contact: T. N. Tiegs, (423) 574-5173 LoTEC, Inc. Contact: Santosh Limaye, (801) 277-6940 In silicon nitride, acicular or elongated grains can be generated by in situ growth and these can provide The overall objective of this effort is to develop sodium- significant toughening on the same order as the zirconium-phosphate (NZP) ceramic-based, "cast-in- whisker-toughened materials. Microstructural place," diesel-engine portliners. Specific objectives are: development to promote growth of in situ toughened (1) development and optimization of the overall microstructures in silicon nitride is the current emphasis insulation system, (2) refinement of the compliant layer of this project. formation process around the ceramic insulation system, (3) development and adaptation of cost- Keywords: Alumina, Composites, Silicon Carbide, effective powder and material fabrication processes; SiAION, Toughened Ceramics and (4) creation of a database of high-temperature properties (stability in diesel exhaust environment, 120. CHARACTERIZATION/TESTING OF LOW CTE thermal cycling, thermal shock, etc.). LoTEC will MATERIALS continue to develop and scale up production of sodium- $100,000 zirconium-phosphate (NZP) materials developed at DOE Contact: Sidney Diamond, (202) 586-8032 Penn State University. ORNL Contact: D. R. Johnson, (423) 576-6832 ORNL Contact: D. P. Stinton, (423) 574-4556 Keywords: Structural Ceramics, Ultra-low Expansion, Zirconia Insulated exhaust portliners are needed in advanced diesel engines to increase engine fuel efficiency by 122. LOW COST NZP POWDER increasing the combustion temperatures and reducing $0 the combustion heat that is lost through the head and DOE Contact: Sidney Diamond, (202) 586-8032 into the water cooling system. Low-expansion materials ORNL Contact: D.R. Johnson, (423) 576-6832 have potential for this application due to their very low LoTEC, Inc. Contact: Santosh Limaye, thermal conductivity, extraordinary thermal-shock (801) 277-6940 resistance, and reduction of attachment stresses. Thermal-shock resistance is critical because the shape The overall objective of this work is to develop a of the portliners requires that they be cast into the suitable technology for low-cost synthesis and metallic cylinder head. Functioning exhaust portliners processing of NZP materials. The two NZP materials of are inaccessible after they are cast into cylinder heads primary interest are BS-25 (Ba 5Zr 4Si05P5.O 24) and and, hence, must not require maintenance for the life of CS-50 (Ca. 5Sr0.5Zr4P6O24). Specific objectives to be the head (- 1 million miles). A contract has been placed accomplished are: (1) preliminary assessment of with LoTEC to develop cost-effective processes for the powder techniques of specialist vendors for cost- fabrication of the portliners. LoTEC is investigating effective NZP powder synthesis; (2) evaluation of NZP Ba,1 Zr4P6.SixO24 (BaZPS) and Cax SrxZr4P6O24. powder samples for phase and impurity content, particle ORNL is assisting with the characterization and size and distribution, surface area, thermal stability, evaluation of the LoTEC compositions. dispersability, flowability, sinterability after green* forming, and synthesis costs; (3) selection of up to two Keywords: Physical/Mechanical Properties, Structural finalist powder suppliers based on results of initial Ceramics, Ultra-low Expansion, Zirconia evaluation, commercial viability of the process, and scale-up costs; (4) advanced evaluation of powders supplied by two companies based on results of material properties testing such as thermal expansion, strength, elastic modulus, etc.; and (5) metal-casting trials involving NZP prototype parts and testing of the

51 Office of Transportation Technologies prototypes for diesel-engine worthiness. A secondary 125. INSULATING STRUCTURAL CERAMICS FOR objective will be to set up a hydrothermal (or other) low- HIGH EFFICIENCY, LOW EMISSION ENGINES cost powder synthesis facility at LoTEC as a parallel $0 effort. DOE Contact: Sidney Diamond, (202) 586-8032 ORNL Contact: D. R. Johnson, (423) 576-6832 Keywords: Powder Characterization, Powders, Caterpillar Contact: Michael Haselkorn, Structural Ceramics, Ultra-low Expansion, (309) 578-2953 Zirconia The overall objective of this new program is to develop 123. ADVANCED MANUFACTURING OF DIESEL a commercially viable, zirconia-toughened mullite ENGINE TURBOROTORS cylinder-head insert for advanced diesel engines using $0 an innovative tape cast and pressureless sintering DOE Contact: Sidney Diamond, (202) 586-8032 process. ORNL Contact: D. R. Johnson, (423) 576-6832 Kyocera Contact: E. Kraft, (206) 750-6147 Keywords: Ceramics, Components, Diesel, Engines, Mullite, Zirconia The objective of this program is to develop the cost- effective manufacturing technology required for ceramic 126. THICK THERMAL BARRIER COATINGS turbine rotors for use in turbochargers for heavy duty (TTBCs) FOR LOW EMISSIONS, HIGH diesel truck and bus applications. A team, led by EFFICIENCY DIESEL ENGINE COMPONENTS Kyocera and including Schwitzer U.S., Inc. and $0 Caterpillar Inc., will develop and demonstrate DOE Contact: Sidney Diamond, (202) 586-8032 production readiness for reliable, cost-affordable, ORNL Contact: D. R. Johnson, (423) 576-6832 turbochargers with ceramic turborotors. Program goals Caterpillar Contact: M. Brad Beardsley, include a nominal order of magnitude reduction in cost (309) 578-8514 over the present cost for small quantities, and process capability for critical component attributes which is The objective of this new program is to develop durable, adequate for the performance and reliability thick thermal barrier coating (TTBC) technologies for specifications of the application, higher efficiency and lower-emission heavy duty diesel engines. Keywords: Components, Cost-Effective Ceramics, Process Control, Silicon Nitride Keywords: Ceramics, Coatings and Films, Components, Diesel, Engines 124. ADVANCED MANUFACTURING OF CERAMIC EXHAUST VALVES FOR DIESEL ENGINES 127. MATERIALS FOR LOW EMISSIONS, HIGH $0 EFFICIENCY DIESEL ENGINE COMPONENTS DOE Contact: Sidney Diamond, (202) 586-8032 $0 ORNL Contact: A. E. Pasto, (423) 574-4956 DOE Contact: Sidney Diamond, (202) 586-8032 Norton Contact: Vimal Pujari, (508) 351-7929 ORNL Contact: D. R. Johnson, (423) 576-6832 Cummins Contact: Paul Becker, The objectives of this program are to design, develop, (812) 377-4701 and demonstrate advanced manufacturing technology for the production of ceramic valves. A production The goal of this new program is to develop advanced manufacturing process for a ceramic exhaust valve for material applications in diesel engine components to DDC's Series 149 diesel engine is being developed enable the design of cleaner, more efficient engines. under this program. Specific objectives are to: Advanced materials may include ceramics, intermetallic (1) reduce manufacturing costs by at least an order of alloys, advanced metal alloys, or ceramic or metal magnitude over current levels; (2) develop and coatings. Components may include in-cylinder demonstrate performance ratio values of 0.7 or less for components, valve-train components, fuel-system all critical component attributes; and (3) to validate components, exhaust system components, and air ceramic valve performance, durability, and reliability in handling systems. rig and engine testing. Keywords: Alloys, Ceramics, Coatings and Films, Keywords: Components, Cost-Effective Ceramics, Components, Diesel, Engines, Process Control, SiAION Intermetallics

52 Office of Transportation Technologies

128. MATERIALS FOR LOW EMISSIONS, HIGH 131. LIFE PREDICTION VERIFICATION EFFICIENCY DIESEL ENGINE COMPONENTS $200,000 $0 DOE Contact: Sidney Diamond, (202) 586-8032 DOE Contact: Sidney Diamond, (202) 586-8032 ORNL Contact: D. R. Johnson, (423) 576-6832 ORNL Contact: D. R. Johnson, (423) 576-6832 ORNL Contact: A. A. Wereszczak, Detroit Diesel Contact: Yuri Kalish, (423) 574-7601 (313) 592-7825 The first goal of this research program is to generate In this program, DDC will investigate the feasibility of engineering data from ambient to high-temperature using a smart-materials-based actuator in place of a mechanical testing of silicon nitride and SiAION. The solenoid for fuel injection actuation. second is to characterize the evolution and role of damage mechanisms using metallography, SEM, and Keywords: Alloys, Ceramics, Coatings and Films, TEM. Lastly, available analytical and numerical models Components, Diesel, Engines, will be utilized to predict the life of complex-shaped Intermetallics components and prototype engine parts (e.g., valves).

129. HIGH STRENGTH MATERIALS FOR DIESEL Keywords: Components, Engines, Failure Analysis, ENGINE FUEL INJECTORS Failure Testing, High Temperature Service, $0 Life Prediction, Mechanical Properties, DOE Contact: Sidney Diamond, (202) 586-8032 Structural Ceramics, Tensile Testing, ORNL Contact: R. L. Beatty, (423) 574-4536 SiAION, Silicon Nitride Cummins Contact: Thomas Yonushonis, (812) 377-7078 132. HIGH TEMPERATURE TENSILE TESTING $250,000 The objective of this new program is to develop DOE Contact: Sidney Diamond, materials for next-generation diesel fuel injectors. (202) 586-8032 ORNL Contact: D. R. Johnson, (423) 576-6832 Keywords: Ceramics, Cermets, Components, Diesel North Carolina A&T State University Contact: J. Sankar, (919) 334-7620 MATERIALS PROPERTIES, BEHAVIOR, CHARACTERIZATION OR TESTING The objective of this research is to test and evaluate the long-term mechanical reliability of Si3N4 at high 130. DIESEL EXHAUST CATALYST temperatures. Microstructural/microchemical analysis of CHARACTERIZATION the fracture surfaces using scanning electron $200,000 microscopy (SEM), transmission electron microscopy DOE Contact: Sidney Diamond, (202) 586-8032 (TEM), and energy-dispersive spectral analysis (EDS) is ORNL Contact: D. R. Johnson, (423) 576-6832 an integral part of this effort. ORNL Contact: L F. Allard, (423) 574-4981 Keywords: Creep, Fracture, Microscopy, Silicon The purpose of this work is to use analytical and high- Nitride, Tensile Testing resolution electron microscopy to characterize the microstructures of emission control catalysts. Emphasis 133. COMPUTED TOMOGRAPHY is placed on relating microstructural changes to $120,000 performance of diesel oxidation catalysts. DOE Contact: Sidney Diamond, (202) 586-8032 ORNL Contact: D. R. Johnson, (423) 576-6832 Keywords: Catalyst Performance, Catalysts, Diesel, Argonne National Lab Contact: W. A. Ellingson, Microstructure, Chemical Analysis, (312) 972-5068 Mechanical Properties, Scanning Electron Microscopy The objective of this project has been redefined to study 3D X-ray CT densitometry reliability relative to detection of density variations in GS-44 with chopped carbon fibers. GS-44 with chopped carbon fibers is being developed as a material for valve guides as part of an effort with Caterpillar. Current processing technology is

53 Office of Transportation Technologies via cold isostatic pressing. Other, more-cost-effective prioritize and implement a long-range research and processing methods may be assessed and a non- development program. destructive method to establish carbon fiber distribution would be highly desirable. Keywords: AGT, Advanced Heat Engines, Coordination, Diesel, Management, Keywords: Carbon Fibers, Components, Computed Structural Ceramics Tomography, Diesel, Engine, Nondestructive Evaluation 137. INTERNATIONAL EXCHANGE AGREEMENT (IEA) 134. ON-MACHINE INSPECTION $200,000 $0 DOE Contact: Sidney Diamond, (202) 586-8032 DOE Contact: Sidney Diamond, (202) 586-8032 ORNL Contact: D. R. Johnson, (423) 576-6832 ORNL Contact: D. R. Johnson, (423) 576-6832 ORNL Contact: M. K. Ferber, (423) 576-0818 Caterpillar Contact: M. K. Haselkorn, (309) 578-6224 The purpose of this effort is to organize, assist, and facilitate international research cooperation on the The primary objective of this new program is to characterization of advanced structural ceramic establish a correlation between nondestructive materials. A major objective of this research is the evaluation techniques and the properties and evolution of measurement standards. Participants in performance of machined ceramic surfaces. Annex II are the United States, Germany, Sweden, Japan, and Belgium. Current research is focused on Keywords: Machining, Nondestructive Evaluation, Subtask 9, Thermal Shock, and Subtask 10, Ceramic Structural Ceramics Powder Characterization.

135. MECHANICAL PROPERTIES OF CMZP Keywords: IEA, Powder Characterization $0 DOE Contact: Sidney Diamond, (202) 586-8032 138. STANDARD REFERENCE MATERIALS ORNL Contact: D. R. Johnson, (423) 576-6832 $200,000 Caterpillar Contact: M. K. Haselkorn, DOE Contact: Sidney Diamond, (202) 586-8032 (309) 578-6624 ORNL Contact: D. R. Johnson, (423) 576-6832 NIST Contact: G. Onoda, (301) 975-4489 The primary objective of this program is to determine the effect of long-term exposure to a diesel-engine- This objective of this project is to tighten and finalize exhaust environment of a particular low-expansion procedures for the characterization of secondary ceramic known as calcium magnesium zirconium properties of powders. There are four focus areas phosphate (CMZP). relating to the secondary properties: dispersion of powders from slurry preparation, slurry preparation, Keywords: CMZP, Diesel, Engine, spray-dried powders, and green body evaluation. Physical/Mechanical Properties, Stability Keywords: IEA, Reference Material, Powder TECHNOLOGY TRANSFER AND MANAGEMENT Characterization COORDINATION 139. MECHANICAL PROPERTY STANDARDIZATION 136. TECHNICAL PROJECT MANAGEMENT $100,000 $565,000 DOE Contact: Sidney Diamond, (202) 586-8032 DOE Contact: Sidney Diamond, (202) 586-8032 ORNL Contact: D. R. Johnson, (423) 576-6832 ORNL Contact: D. R. Johnson, (423) 576-6832 NIST Contact: G. Quinn, (301) 975-5765

The objective of this effort is to assess the materials The purpose of this effort is to develop mechanical test technology needs for high-efficiency diesel engines, standards in support of the Heavy Vehicle Propulsion formulate technical plans to meet these needs, and System Materials Program.

Keywords: Mechanical Properties, Test Procedures

54 Office of Transportation Technologies

DEVICE OR COMPONENT FABRICATION, 142. ADVANCED MACHINING/MANUFACTURING BEHAVIOR OR TESTING $223,000 DOE Contact: Sidney Diamond, (202) 586-8032 140. THICK THERMAL BARRIER SEAL COATINGS ORNL Contact: D. R. Johnson, (423) 576-6832 $33,000 ORNL Contact: S. B. McSpadden, Jr., DOE Contact: Sidney Diamond, (202) 586-8032 (423) 574-5444 ORNL Contact: D. R. Johnson, (423) 576-6832 ORNL Contact: D. P. Stinton, (423) 574-4556 The objective of this effort is to develop and demonstrate optimized grinding processes for the The purpose of this exploratory research program was production of difficult-to-machine components for use in to assess the possibility for sealing the surface of diesel engines. porous thermal barrier coatings (TBCs) with a thin oxide

coating prepared by chemical vapor deposition. A12 03 , Keywords: Cost-Effective Ceramics, Machining, SiO2, mullite, and ZrO2 were evaluated as candidate Silicon Nitride, Structural Ceramics seal coating materials. The high-temperature stability of the sealed TBC structures was studied by performing 143. NEXT-GENERATION GRINDING WHEEL cyclic oxidation experiments at ORNL and gas $0 permeability measurements at Caterpillar. DOE Contact: Sidney Diamond, (202) 586-8032 ORNL Contact: P. J. Blau, (423) 574-5377 Keywords: Coatings, Chemical Vapor Deposition, Norton Contact: Robert H. Licht, CVD, Diesel, Engines, Thermal Barrier (508) 351-7815 Coatings This effort is aimed at the engineering design and 141. CHARACTERIZATION OF MACHINED development of a next-generation, superabrasive CERAMICS grinding wheel specifically tailored for the cylindrical $200,000 grinding of silicon nitride and other advanced structural DOE Contact: Sidney Diamond, (202) 586-8032 ceramic parts for automotive and truck engine ORNL Contact: D. R. Johnson, (423) 576-6832 applications. The intent of this effort is to significantly ORNL Contact: P.J. Blau, (423) 574-5377 reduce manufacturing cost of ceramic parts and to enhance the competitiveness of U.S. industry by The purpose of this task was to develop, in conjunction providing an optimized grinding wheel for ceramics. The with U.S. industry, advanced technologies and the Phase I objectives to define requirements, and design, associated scientific and economic concepts necessary develop, and evaluate a next-generation grinding wheel to reduce the costs for machining of structural ceramics for cost-effective cylindrical grinding of advanced for energy-efficient, low-emissions transportation ceramics have been met. The overall objectives of the systems. This effort was conducted by industry, other Phase II effort are: (1) to scale up the manufacturing national laboratories, and in-house at ORNL. The ORNL process for the Phase I experimental wheel composition research concerned two technical areas: 1) investigating in order to manufacture 356-mm- (14-in.-) diameter the effects of machining practices on the durability of grinding wheels; and to validate the performance of the ceramics for valve and valve-seat applications; and 2) new wheels in cylindrical grinding of advanced ceramics understanding and characterizing the detailed nature of at independent test sites. machining-induced surface and subsurface damage and their evolution in advanced ceramic materials using a Keywords: Cost-Effective Ceramics, Machining, range of analytical tools. Silicon Nitride, Structural Ceramics, Surface Characterization and Treatment Keywords: Cost-Effective Ceramics, Machining, Silicon Nitride, Structural Ceramics 144. HIGH SPEED GRINDING $0 DOE Contact: Sidney Diamond, (202) 586-8032 ORNL Contact: P.J. Blau, (423) 574-5377 Eaton Contact: Joseph A Kovach, (216) 523-6766

The purpose of this effort is to develop a single step, rough finishing process suitable for producing high- quality silicon nitride ceramic parts at high material

55 Office of Transportation Technologies removal rates and at substantially lower cost than 147. NEXT GENERATION GRINDING SPINDLE traditional, multi-stage grinding processes. Initial $0 implications from Phase I have suggested that HSLD DOE Contact: Sidney Diamond, (202) 586-8032 grinding of Si3N4 is technically feasible. Accordingly, the ORNL Contact: P. J. Blau, (423) 574-5377 Phase II effort is focused on: (1) continued expansion of Eaton Contact: J. A. Kovach, (216) 523-6766 the HSLD science base; (2) further development of the enabling HSLD technologies required for successful The objective of this effort is to design, develop, test, implementation; and (3) economic analysis of the HSLD and demonstrate the operation of a next generation, production cost drivers. high-stiffness, high-speed spindle to be used for centerless grinding of ceramic parts. Keywords: Cost-Effective Ceramics, Machining, Silicon Nitride, Structural Ceramics, Keywords: Machining, Structural Ceramics Surface Characterization and Treatment 148. PROCESS COST MODEL 145. LASER-BASED NDE METHODS $0 $80,000 DOE Contact: Sidney Diamond, (202) 586-8032 DOE Contact: Sidney Diamond, (202) 586-8032 ORNL Contact: S. G. Winslow, (423) 574-0965 ORNL Contact: D. R. Johnson, (423) 576-6832 AlliedSignal Ceramic Components Contact: Argonne National Lab Contact: J. G. Sun, J. M. Wimmer, (312) 512-3183 (708) 252-5169 The objective of this effort was to refine and utilize a The primary objective of this program is to develop a process cost model for the evaluation of various laser-based, elastic optical scattering procedure which fabrication methods used to manufacture diesel engine would provide a direct (near-real-time) method to detect and aerospace/industrial turbomachinery structural machining-induced damage in monolithic ceramics. ceramic components and provide a report containing an Median and lateral crack detection are of primary analysis of the process cost modeling effort. importance. The laser-based elastic optical scattering program is being executed in three steps. The first is to Keywords: Cost-Effective Ceramics, Cost Reduction, optimize the elastic scattering procedure by examining Modeling, Processing, Structural Ceramics specimens machined using innovative machining techniques. The second step involves correlation of the 149. INTELLIGENT GRINDING WHEEL elastic scattering results with mechanical properties in $0 "real' machined ceramic specimens. The final step DOE Contact: Sidney Diamond, (202) 586-8032 involves the development of a prototype instrument to ORNL Contact: P. J. Blau, (423) 574-5377 be evaluated for on-line implementation in a production University of Massachusetts Contact: environment. Stephen Malkin, (413) 545-3687

Keywords: Machining, Nondestructive Evaluation, The objective of this effort is to develop an 'intelligent Structural Ceramics grinding wheel" for in-process monitoring of ceramic grinding processes. Such a wheel will be smart enough 146. GRINDING MACHINE STIFFNESS to monitor its 'state" or condition" during truing, $0 dressing, and grinding; to identify the prevailing grinding DOE Contact: Sidney Diamond, (202) 586-8032 mechanisms (ductile versus brittle); and to use this real- ORNL Contact: P.J. Blau, (423) 574-5377 time information as a feedback signal for process University of Connecticut Contact: Bi Zhang, control and optimization. In order to monitor the wheel (203) 486-3576 working condition and the grinding processes in a real- time and on-line fashion, without additional instrumenta- The objective of this effort is to determine the minimum tion, both acoustic emission sensors and dynamic force required grinding machine stiffness to meet acceptable sensors, together with the primary signal-processing quality requirements for ground silicon nitride ceramic electronics, will be embedded in the core of the grinding parts. wheel.

Keywords: Machining, Silicon Nitride Keywords: Cost-Effective Ceramics, Machining, Structural Ceramics

56 Office of Utility Technologies

OFFICE OF UTILITY TECHNOLOGIES

FY 1997

Office of Utility Technologies - Grand Total $38,810,000

Office of Solar Energy Conversion $18,460,000

Photovoltaic Eneray Technoloyv Division $18,460,000

Materials Preparation. Synthesis. Deposition. Growth or Forming $12,800,000

Amorphous Silicon for Solar Cells 3,370,000 Polycrystalline Thin Film Materials for Solar Cells 8,110,000 Deposition of III-V Semiconductors for High-Efficiency Solar Cells 1,320,000

Materials Properties. Behavior. Characterization or Testing $ 3,550,000

Materials and Device Characterization $ 3,550,000

Device or Component Fabrication. Behavior or Testing $ 2,110,000

High-Efficiency Crystalline Silicon Solar Cells 2,110,000

Office of Geothermal Technologies $ 600,000

Materials Preparation. Synthesis. Deposition. Growth or Forming $ 125,000

Thermally Conductive Composites for Heat Exchangers 125,000

Materials Properties. Behavior. Characterization or Testing $ 475,000

Advanced High Temperature Geothermal Well Cements 125,000 Corrosion Mitigation at The Geysers 100,000 Advanced Coating Materials 100,000 Thermally Conductive Cementitious Grouts for Geothermal Heat Pumps 150,000

Office of Eneray Management $19,750,000

Advanced Utility Concepts Division $19,750,000 High Temperature Superconductivity for Electric Systems $19,750,000

Device or Component Fabrication. Behavior or Testing $19,750,000

Wire Technology 5,000,000 Systems Technology 5,250,000 Superconductivity Partnership Initiative 9,500,000

57 Office of Utility Technologies

OFFICE OF UTILITY TECHNOLOGIES

OFFICE OF SOLAR ENERGY CONVERSION

PHOTOVOLTAIC ENERGY TECHNOLOGY DIVISION

The National Photovoltaics program sponsors high-risk, potentially high-payoff research and development in photovoltaic energy technology that will result in a technology base from which private enterprise can choose options for further development and competitive application in U.S. electrical markets. The objective of materials research is to overcome the technical barriers currently limiting the efficiency and cost of photovoltaic cells. Theoretical conversion efficiency of photovoltaic cells is limited by the portion of the solar spectrum to which the cell's semiconductor material can respond, and by the extent to which these materials can convert each photon to electricity. The practical efficiency is constrained by the amount of light captured by the cell, the cell's uniformity, and a variety of loss mechanisms for the photo- generated carriers. Cost is affected by the expense and amount of materials required, the complexity of processes for fabricating the appropriate materials, and the complexity and efficiency of converting these materials into cells and modules.

MATERIALS PREPARATION, SYNTHESIS, cells. Research centers upon improving solar cell DEPOSITION, GROWTH OR FORMING conversion efficiency by depositing more nearly stoichiometric films, by controlling interlayer diffusion 150. AMORPHOUS SILICON FOR SOLAR CELLS and lattice matching in heterojunction structures and by $3,370,000 controlling the uniformity of deposition over large DOE Contact Jeffrey Mazer: (202) 586-2455 (4000 cm2) areas. The films are deposited by chemical NREL Contact: Bolko von Roedern, and physical vapor deposition, electrodeposition and (303) 384-6480 sputtering. The long term goal of this effort is to develop the technology for 15 percent efficient photovoltaic This project performs applied research upon the modules with cost under $50/m2and with 30-year deposition of amorphous silicon alloys to improve solar lifetime. This will allow an entire system lifetime energy cell properties. Efficient solar energy conversion is cost of under $0.06/kWh. Achieving this goal will hindered by improper impurities or undesired structure enable polycrystalline thin film material to be a cost- in the deposited films and the level of uniformity of the effective utility-scale generator. films over large (4000 cm2) areas. The films are deposited by plasma enhanced chemical vapor Keywords: Coatings and Films, Semiconductors, deposition (glow discharge), thermal chemical vapor Chemical Vapor Deposition, Physical deposition and sputtering. The long term goal of this Vapor Deposition, Electrodeposition, effort is to develop the technology for 15 percent Sputtering, Solar Cells efficient photovoltaic modules with cost under $50/m2 and with 30-year lifetime. This will allow an entire 152. DEPOSITION OF III-V SEMICONDUCTORS FOR system lifetime energy cost of under $0.06/kWh. HIGH-EFFICIENCY SOLAR CELLS Achieving that goal will enable amorphous silicon to be $1,320,000 a cost-effective utility-scale generator. DOE Contact: Jeffrey Mazer, (202) 586-2455 NREL Contact: John Benner, (303) 384-6496 Keywords: Amorphous Materials, Coatings and Films, Semiconductors, Chemical Vapor This project performs applied research upon deposition Deposition, Sputtering, Solar Cells of III-V semiconductors for high efficiency solar cells, both thin film for flat plate applications and multilayer 151. POLYCRYSTALLINE THIN FILM MATERIALS cells for concentrator applications. Research centers FOR SOLAR CELLS upon depositing layers precisely controlled in terms of $8,110,000 composition, thickness and uniformity and studying the DOE Contact: Jeffrey Mazer, (202) 586-2455 interfaces between the layers. The materials are NREL Contact: Kenneth Zweibel, (303) 384-6441 deposited by chemical vapor deposition, liquid phase epitaxial growth and molecular beam epitaxial growth. This project performs applied research upon the The long term goal of this area is to develop 35 percent deposition of CulnSe2 and CdTe thin films for solar efficient concentrator cells and 24 percent efficient 100 cm2 one-sun cells for flat plate applications.

58 Office of Utility Technologies

Achieving these goals will enable systems using these photolithography-free protocol that will yield 18 percent technologies to be cost-effective utility-scale efficient 100 cm 2cells on multi-crystalline material in a generators. commercial production environment.

Keywords: Semiconductors, Chemical Vapor Keywords: Semiconductors, Solar Cells, Crystal Silicon Deposition, Solar Cells OFFICE OF GEOTHERMAL TECHNOLOGIES MATERIALS PROPERTIES, BEHAVIOR, CHARACTERIZATION OR TESTING The primary goal of the geothermal materials program is to ensure that the private sector development of 153. MATERIALS AND DEVICE geothermal energy resources is not constrained by the CHARACTERIZATION availability of technologically and economically viable $3,550,000 materials of construction. This requires the performance DOE Contact: Jeffrey Mazer, (202) 586-2455 of intermediate and long-term high risk OGT-sponsored NREL Contact: Larry Kazmerski, (303) 384-6600 materials research and development.

This project measures and characterizes materials and MATERIALS PREPARATION, SYNTHESIS, device properties. The project performs surface and DEPOSITION, GROWTH OR FORMING interface analysis, electro-optical characterization and cell performance and material evaluation to study 155. THERMALLY CONDUCTIVE COMPOSITES critical material/cell parameters such as impurities, FOR HEAT EXCHANGERS layer mismatch and other defects that limit performance $125,000 and lifetime. Techniques that are used include deep DOE Contact: R. LaSala, (202) 5864198 level transient spectroscopy, electron beam induced BNL Contact: M. L. Allan, (516) 344-3060 current, secondary ion mass spectroscopy, scanning electron microscopy and scanning transmission electron This project is investigating thin thermally conductive microscopy. polymer-based composites for use as corrosion and scale-resistant liner materials on carbon steel tubing Keywords: Semiconductors, Nondestructive used in shell and tube heat exchangers in binary Evaluation, Surface Characterization, geothermal processes or for bottoming cycles in multi- Microstructure, Solar Cells stage flash plants. Corrosion and scaling on the brine side of carbon steel tubing in shell and tube heat DEVICE OR COMPONENT FABRICATION, exchangers have been major problems in the operation BEHAVIOR OR TESTING of geothermal processes. Compared to the cost of high alloy steels, a considerable economic benefit could 154. HIGH-EFFICIENCY CRYSTALLINE SILICON result from the utilization of a proven corrosion resistant SOLAR CELLS composite material if sufficient heat transfer and anti- $2,110,000 fouling properties can be achieved. The work consists of DOE Contact: Jeffrey Mazer, (202) 586-2455 determination of the effects of compositional and NREL Contact: John Benner, (303) 384-649 processing variables on the thermal and fouling SNL Contact: Margie Tatro, (505) 844-3154 properties of the composite and measurements of the physical and mechanical properties after exposure to This project performs applied research upon crystalline hot brine in the laboratory and in plant operations. The silicon devices to improve solar-to-electric conversion effects of antioxidant, SiC fillers and low surface energy efficiency. The project employs new and improved additives on the fouling coefficient and scale adhesion dopant profiles, back-surface fields, and bulk passiva- are also being evaluated. tion treatments to reduce electron-hole recombination at cell surfaces and in the bulk. Control of point defects in Fundamental work to elucidate the interactions that take crystalline silicon is being studied by a variety of place at the thermally conductive composite/ scale techniques, and is thoroughly discussed at the annual interface was performed. The results of these studies NREL-sponsored Silicon Defects Conference. indicated that polymers containing ester, ketone or ether Additionally, improved light-trapping surface treatments functional groups should not be used as liner materials for thin cells (-50 to 100 microns thick), and improved because of their susceptibility to oxidation reactions with methods for inexpensive silver-paste contact screen hot brine. This reaction led to formation of carboxylic printing are also under development. One of the major acid groups which subsequently react with Ba and Ca in goals of this project is to develop a rapid-thermal- geothermal brines. The Ba- and Ca-complexed processing (RTP)-based, screen-printed-contact, carboxylate salt derivatives not only acted to promote

59 Office of Utility Technologies

the rate of scale deposition, but also caused the resistant to brines containing high concentrations of development of high bond strength at the interfaces CO2 at temperatures >150°C are also needed. between the coating and scale. Based on these findings, Emphasis is being placed on high temperature the incorporation of antioxidants and the use of polyaryl rheology, phase chemistry, and the mechanical, type polymers were selected for field testing. physical, and chemical resistance properties of the cured materials. Retarding admixtures required to Field tests with flowing hypersaline brine under heat maintain pumpability during placement operations are exchange conditions in conjunction with NREL are in also being identified. progress to evaluate the following coatings. Cost-shared R&D between BNL, Halliburton Services * Styrene/TMPTMA/SiC/antioxidant and Unocal to develop cementing materials produced by acid-base reactions between fly ash-blended calcium · Styrene/TMPTMA/SiC aluminate cements and phosphate-containing compounds was continued. Several candidate systems were * Styrene/TMPTMA/SiC/antioxidant over zinc evaluated. Studies of the cementing phases formed, phosphate microstructure developed, carbonation rate, and changes in strength and permeability after exposure to * Styrene/TMPTMA/SiC over zinc phosphate CO2 solutions at 3000C were completed. As a result, a formulation was tentatively selected for use in a full- * Polyphenylene sulfide over zinc phosphate scale test performed in FY 1997. The basic cement formulation consists of 23.7 wt% fly ash; 15.8 wt% * Polyphenylene sulfide/SiC over zinc phosphate calcium aluminate cements, 12.6 wt% sodium polyphosphate, 29.1 wt% A120 3-shelled microspheres, Preliminary results indicate a trend for the coats and 18.8 wt% water. This formulation has a slurry containing antioxidants to have greater fouling density of approximately 1.2 g/cc, and after resistance. If this behavior is sustained the coatings will hydrothermal curing forms a strong, CO2-resistant represent a significant advancement in overcoming cement. As an example, autoclave exposure for 120 problems of both corrosion and scale resistance. days to a 4 wt% Na2CO3 solution at 300°C produced no Research is also underway to improve methods of evidence of carbonation or strength retrogression. In attaching the lined heat exchanger tubes to tube sheets. contrast, Class G cement that is conventionally used for The results from preliminary design, manufacturing and geothermal well completions was severely deteriorated. cost studies indicate that contingent upon the develop- A production well in. Indonesia was recently successfully ment of a method for joining the composite lined tubes completed with the developed calcium phosphate to the tube sheets, reductions in the cost of heat cement and use of this material in two more wells in exchangers up to 65% could be realized. 1998 is planned.

Keywords: Composites, Polymers, Corrosion, Heat Keywords: Cements, Material Degradation, Strength, Transfer, Heat Exchanger Tubes, Scale- Drilling, Carbonation, Retarders, Well Resistant, Fabrication Technology, Fouling Completions Coefficient 157. CORROSION MITIGATION AT THE GEYSERS MATERIALS PROPERTIES, BEHAVIOR, $100,000 CHARACTERIZATION OR TESTING DOE Contact: R. LaSala, (202) 586-4198 BNL Contact: M. L. Allan, (516) 344-3060 156. ADVANCED HIGH TEMPERATURE GEOTHERMAL WELL CEMENTS Increased HCI gas concentrations in the steam $125,000 produced from geothermal wells at The Geysers in DOE Contact: R. LaSala, (202) 586-4198 Northern California have resulted in severe corrosion BNL Contact: M. L. Allan, (516) 344-3060 problems in casings in the upper regions of wells where condensation may occur, in the well-head, transmission Lightweight (<1.2 g/cc), environmentally benign, piping, turbines, and cooling towers. The objective of chemically and thermally resistant well cements are the program is to optimize and field test polymers, needed to reduce the potential for lost circulation polymer matrix composites, and ceramic matrix problems during well completion operations and to composites for utilization as corrosion resistive liners on ensure long-term well integrity. Materials designed for components exposed to low pH steam condensates at temperatures >400°C will be needed as higher temperatures up to -200°C. The identification of need, temperature resources are developed. Cements performance of prototype and full-scale field evaluations, and subsequent economic studies are

60 Office of Utility Technologies performed as cost-shared activities with firms active at tests were also conducted to determine the possibility of The Geysers. using the coatings in conjunction with cathodic protection. In FY 1997, a number of potential coating systems were developed by BNL and were investigated in laboratory- It was found that the tested coatings were resistant to scale work. These included: (a) refractory oxides (ZrO2, chemical attack and biodegradation at the test Al203, and Y203), (b) ceramic-sealed NiAI alloy compo- temperature of 55°C. The thermal sprayed ethylene sites, (c) fly ash-derived glass ceramics and (d) PPS- methacrylic acid coatings protected 316L stainless steel sealed NiAI alloy composites. These materials were from corrosion in coupon tests. However, corrosion of evaluated for use as corrosion/oxidation/abrasion- mild steel substrates coated with ethylene methacrylic resistant coatings for mild carbon steel, stainless steel, acid and ethylene tetrafluoroethylene occurred in Atlas Ni-Cr steel and Ti-based alloys, cell tests that simulated a lined reactor operating environment, and this resulted in decreased adhesive Keywords: Corrosion Protection, Polymers, strength. The ceramic-filled epoxy performed well with Composites, Ceramics, Well Casing, only slight substrate corrosion occurring after 18 weeks Turbine Components, Piping, Acid of exposure. This coating also displayed excellent Condensate abrasion resistance and is recommended for further testing in pilot-scale biochemical processing equipment. 158. ADVANCED COATING MATERIALS $100,000 Keywords: Corrosion Protection, Polymers, DOE Contact: R. LaSala, (202) 586-4198 Composites, Biochemical Processes, BNL Contact: M. L. Allan, (516) 344-3060 Thermal Spraying, Adhesion, Cathode Protection Corrosion of plant components is a problem that is encountered in most geothermal processes, and low 159. THERMALLY CONDUCTIVE CEMENTITIOUS cost solutions are needed in order to maintain the GROUTS FOR GEOTHERMAL HEAT PUMPS economic competitiveness of this large and $150,000 environmentally benign energy source. The objective of DOE Contact: R. LaSala, (202) 586-4198 this task is to optimize and field test polymers and BNL Contact: M. L. Allan, (516) 344-3060 polymer, ceramic, and metal composites, developed in other parts of the Geothermal Materials Development Ground head exchangers used with geothermal heat Program, as corrosion protective systems for use in pumps (GHPs) rely on a backfill material to provide brine dominated geothermal electric generation heat transfer between the polyethylene U-tube and processes and for the biochemical treatment of plant surrounding formation. Critical properties of the backfill wastes. Successful evaluations and subsequent grout are thermal conductivity, cost, ease of placement, technology transfer will result in reduced plant impermeability, shrinkage resistance, bonding to U-tube construction and operation costs, increased generation and formation, and durability. By increasing the thermal efficiencies and utilization factors, and enhanced conductivity of the grouting material the required length environmental acceptance. of the heat exchanger can be decreased, and this results in decreased installation costs in addition to Thermal sprayed WC-12%Co and Cr3C2-NiCr coatings improved GHP performance. were evaluated for corrosion and erosion protection of vent gas blowers. These coatings are currently In FY 1997 Brookhaven National Laboratory initiated undergoing field tests. Thermal sprayed ethylene research to develop high thermal conductivity tetrafluoroethylene and ethylene methacrylic acid cementitious grouts for geothermal heat pumps. This polymers, spray-and-bake fluoropolymers and research is focused on cement-silica sand grouts. The brushable ceramic-filled epoxy were investigated as effects of sand gradation and proportion on properties coatings to protect mild steel and 316L stainless steel such as thermal conductivity, permeability, shrinkage, from geothermal sludge, synthetic hypersaline brine and coefficient of thermal expansion, bond strength, leach Thiolacillus ferrooxidans at 55°C in laboratory scale resistance and durability have been investigated. tests. All thermal spraying was performed at the State Thermal conductivities between 2.4 and 2.8 W/mK have University of New York at Stony Brook. The coatings been achieved, depending on sand type, content and were selected on the basis of their predicted resistance water/cement ratio. This compares with 0.84 and to chemical attack and biodegradation, ease of large- 0.80 W/mK for neat cement grouts with water/cement scale application, and economics. Long-term exposure ratios of 0.6 and 0.8, respectively. Conventional high tests in simulated environments were conducted and the solids bentonite grout has a thermal conductivity around coatings performance assessed. Residual adhesion 0.75-0.8 W/mK and bentonite-sand grout can be after exposure was measured. Cathodic disbondment

61 Office of Utility Technologies expected to have a value around 1.46 W/mK. Cost The wire technology goal is improvement in short wire analysis and the impact of the developed thermally samples (1 cm to 10 cm) through: improved powder conductive grouts on heat exchanger length design have synthesis, improved fundamental understanding of been conducted in collaboration with the University of critical currents in high temperature superconductors, Alabama. and investigation of new wire processing methods. Improvement in long wire length uniformity is included It is intended to conduct a field trial in FY98 to evaluate in the Systems Technology project below. the developed grout under realistic working conditions, further examine bonding between grout, U-tube and The wire development project is the key to eventual surrounding formation, measure freeze-thaw resistance commercialization of superconductivity systems. of the grouts and investigate non-destructive methods Subtasks in the project are as follows: for detecting loss of bonding in any grouting material. a. Ink development and spray deposition - To Keywords: Geothermal Heat Pumps, Cementitious develop high quality, low cost methods for the Grouts, Backfill, Ground Heat Exchanger, delivery of superconductor precursor materials in Thermal Conductivity a commercially scalable thick-film process using ink-spray techniques. OFFICE OF ENERGY MANAGEMENT b. Thallination and advanced substrate ADVANCED UTILITY CONCEPTS DIVISION development - Continue to optimize the thallination parameters leading to high Jc The Advanced Utility Concepts Division supports superconducting films and develop and evaluate a research and development of advanced energy storage textured substrate to permit the synthesis of a and electrochemical conversion systems that will bi-axially textured oxide film. To scale up the facilitate the substitution of renewable energy sources thallination apparatus to allow longer length for fossil fuels-measures that will increase the reliability development of superconducting samples leading and efficiency of the energy economy. The goal is to eventually to a continuous thallination process. provide reliable, inexpensive devices to mitigate the temporal and spatial mismatches between energy c. Development of Thallium based conductors - The supply and energy demand. purpose of the TI-based conductor development project is to develop materials and processes HIGH TEMPERATURE SUPERCONDUCTIVITY FOR which will lead to the practical production of wires ELECTRIC SYSTEMS and tapes capable of carrying high currents in the presence of typical operating magnetic fields at DEVICE OR COMPONENT FABRICATION, liquid nitrogen temperatures. BEHAVIOR OR TESTING ~~~~BEHAVIORTESTING OR ^d. Practical conductor development for electrical 160. WIRE TECHNOLOGY power systems utilizing high Tc oxides; $5,000,000 characterization of aligned Bi(2223) in AG PIT DOE Contact: Jim Daley, (202) 586-1165 tapes - The purpose of this project is to make Argonne'NationalContact: Laboratory detailed characterization of electrical magnetic Argonne National Laboratory Contact: BalachandraneU. (708) 2524250 properties, such as AC losses and critical

David Welch, (516) 282-3517 critical assessments of the conductors, as well as Los Alamos NationalLos Alamos LaboratoryNational Contact: to provide pertinent data for the design of various Dean Peterson, (505) 665-3030 electrical devices. National Renewable Energy Laboratory of high l and J, BSCCO Contact:ContactiRechardtBaugher, Richard Blaugher, (303)Cconductors 384t518384-6518 e. Development- The main part of the project is aimed Oak Ridge National Laboratory Contact: RobertigNaat Hawsey, (615) 574-8057 understanding the effects of optimal defect RoberSandiaNatinal Labratory Cntact: Peter Rotgeometry and density on the high temperature, Sandia National Laboratory Contact: Peter Roth, field performance of Bi-2223 tapes. The (505) 845-9301845-9301?(505) 'high American Superconductor Contact: G. N. Riley, defects are produced by the recoil of proton (508) 836-4200 induced fission fragments in the Bi-2223 cores of IntermagneticsCo. C General: the tapes, which result in splayed columnar Intermagnetics General Corp. Contact: ft Paradeep Haldar, (518) 782-1122 defects.

62 Office of Utility Technologies f. High rate deposition technology for long-length Systems technology goals include: improved uniformity conductors - The purpose of this project is to in long (10 meter to 1000 meter) high temperature develop metal-organic chemical vapor deposition superconductor (HTS) wires, development of high field processes to fabricate high-quality superconductor (2-5 telsa) coils, and design of high efficiency electric coatings on long-length substrates. Film composi- power devices. tion, crystallinity, morphology, and superconducting properties as a function of chemical The electric power application project includes precursor, gas pressure, flow rate, substrate development of long length wire manufacture and coil materials, and deposition temperatures will be manufacture. Some preliminary systems development systematically investigated. is also done. Project subtasks are as follows: g. High current YBCO coated-conductor a. AC-loss calorimeter system for HTS power trans- development - The objectives of this project mission cables - The objective of this project is to included: Development of continuous processing develop an AC-loss calorimetric measurement of both the IBAD buffer layer and the system capable of determining the total AC-losses laser-deposited YBCO layers at lengths of one (hysteretic eddy current and coupling) of an HTS meter. Investigation of means to accelerate and cable conductor operating in a 3-phase economize the deposition of IBAD layer. environment. Investigation of accelerated deposition of the YBCO layer. b. Practical conductor development for electrical power systems utilizing high Tc oxides: h. Deposited conductors on textured metal characterization of electrical and magnetic substrates - The purpose of the project is to properties - The purpose of this project is: to develop scalable processes for fabrication of make detailed characterization of electrical and conductors for high temperature, high field magnetic properties, such as ac losses and applications The objectives for this project are: To critical currents, of cuprate conductors in order to obtain proof-of-principle for the RABITS make critical assessments of the conductors, as (Rolling-Assisted Biaxially Textured Substrate) well as to provide pertinent data for the design of approach to conductor fabrication by various electrical devices. demonstrating high critical current densities in a reproducible manner. For this purpose, primarily c. Power applications of high temperature pulsed laser deposition has been used for oxide superconductors - To develop HTS components buffer layers and YBa2Cu3O,. relating to electric power applications. Evaluate techniques and approaches to manufacture HTS Keywords: Superconductor, Thallium Conductor, coils and magnets for use in power-related Bismuth Conductor, Coated Conductor applications such as transformers, motors, generators, fault current limiters, SMES and 161. SYSTEMS TECHNOLOGY transmission cable. Manufacture long lengths of $5,250,000 Bi-2223 multi filament conductor and Bi-2212 DOE Contact: Jim Daley, (202) 586-1165 surface-coated conductor for use in the Argonne National Laboratory Contact: demonstration of prototype systems. U. Balachandran, (708) 252-4250 Brookhaven National Laboratory Contact: d. Long-length HTS conductors - The purpose of this David Welch, (516) 282-3517 project is to develop technology to fabricate long- Los Alamos National Laboratory Contact: length conductors with superconducting and Dean Peterson, (505) 665-3030 mechanical properties suitable for commercial National Renewable Energy Laboratory Contact: operation at temperature approaching 77K. Richard Blaugher, (303) 384-6518 Oak Ridge National Laboratory Contact: e. Resistive fault current limiter - The purpose of the Robert Hawsey, (615) 574-8057 project is to develop a resistive 100A fault current Sandia National Laboratory Contact: limiter from sintered YBCO. The device would be Thomas Bickel, (505) 845-9301 an intermediate step in the development of a American Superconductor Contact: G. N. Riley, commercial FCL(600 A/12 kV) for distribution (508) 836-4200 lines of an electric utility. Intermagnetics General Corp. Contact: Paradeep Haldar, (518) 782-1122 f. HTS transmission cable - The purpose of this Oxford Instruments, Inc. Contact: K. R. Marken, project is to develop the technology necessary to (908) 541-1300 proceed to commercialization of high temperature

63 Office of Utility Technologies

superconducting transmission cable. The objec- and a small company supplier of superconducting tives are to design and construct a low-cost, 2000 components. Each team also includes one or more A AC, bare 1 m HTS cable prototype, and test its national laboratories who perform specific tasks defined performance. by the team. The SPI goal is to design cost-effective HTS systems for electricity generation, delivery and g. Conductor, coil, and apparatus development for use. The funding amount below includes the utility and commercial applications - The purpose Department's share of the SPI design activities, as well of this project is to establish the technical and as parallel HTS technology development that directly economic feasibility and benefits to society of HTS supports the SPI teams. In FY 1997, projects are transformers of medium(30 MVA) to large rating. underway for a superconducting fault-current limiter The objective is to design and begin the construc- (Lockheed-Martin), and 100 HP motor (Rockwell tion of a nominal 1 MVA HTS demonstration Automation). In addition, a transmission cable project, transformer incorporating the concepts developed, led by the Electric Power Research Institute and Pirelli Cable, was funded. All of these projects will incorporate high-temperature superconducting wire. Four h. AC wires and AC coils for power applications - Department of Energy National Laboratories are The objective of this AC loss effort is to support currently directly supporting the Superconductivity the development of a high temperature Partnership Projects: Argonne, Los Alamos, Oak Ridge, superconductor developed for AC applications, and Sandia. The low level of loss observed in the experimental data indicated that improvements in the AC Project subtasks are as follows: apparatus would be required to characterize long continuous lengths of conductor. The main a. Fault Current Limiter - The fault current limiter concern was the variation in the field homogeneity project undertook conceptual studies of various for long sample lengths when the sample was device designs, provided a market survey for exposed to AC fields perpendicular to the wide current limiter applications, completed an energy face of the conductor. benefit assessment, conducted a network interface assessment, determined conductor i. High gradient magnetic separation - The objective requirements, and analyzed the economic is to design and build a prototype industrial HTS potential of fault current limiters. Fault current high gradient magnetic separation system. The limiters can be used on transmission and copper coils used in conventional industrial distribution systems to improve system flexibility, magnetic separation systems consume large reliability and performance. amounts of electrical power. Significant energy savings are possible if superconducting magnet Lockheed Martin Contact: Eddie Leung, systems are used. (619) 974-1166

Keywords: Long Length Conductor, Bearing, b. Motor- Electrical and mechanical design and Flywheels, Superconducting Tape, Power thermal analysis was completed. In addition,' the Transmission Cable, Resistive Fault construction of the components for a motor Current Limiter, Magnetic Separation, prototype will be nearly completed, with assembly Transformer and testing. Superconducting motors can have a large impact on electrical energy utilization 162. SUPERCONDUCTIVITY PARTNERSHIP through reduced losses and size compared to INITIATIVE conventional iron core motors. These reduced $9,500,000 losses and the smaller size will be the driving DOE Contact: Chris Platt, (202) 586-4563 force for the commercial introduction of superconducting motors in industrial applications. The Superconductivity Partnership Initiative (SPI) is an industry-led venture between the Department of Energy Rockwell Automation Contact: David Driscoll, and four industrial consortia intended to accelerate the (216) 266-6002 use of high temperature superconductivity in energy applications. Each SPI team includes a vertical c. High Temperature Superconducting Power integration of non-competing companies that represent Cable - The first phase of the contract calls for the the entire spectrum of the R&D cycle. That is, the teams development and fabrication of a 30-meter include the ultimate user of the technology-the electric prototype 115KV HTS underground power utilities-as well as a major manufacturing company transmission cable which will be tested at a utility

64 -- Office of Utility Technologies

test site. Additionally, the project will conclude with design of a 3-phase, 100 meter cable system.

Electric Power Research Institute Contact: Don Von Dollen, (415) 855-2679

Keywords: Motor, Fault Current Limiter, Transmission Cable

65 Office of Energy Research

OFFICE OF ENERGY RESEARCH

FY 1997

Office of Eneray Research - Grand Total $431,936,392

Office of Basic Eneray Sciences $344,107,192

Division of Materials Sciences $332,060,000

Division of Chemical Sciences $ 5,143,000

Division of Engineering and Geosciences $ 6,904,192

Engineerina Sciences Research $ 3,946,973

Materials Preparation. Synthesis. Deposition. Growth or Forming $ 1,0d9,868

Fundamentals of Thermal Plasma Processing 478,000 Multivariable Control of the Gas-Metal Arc Welding Process 153,000 Metal Transfer in Gas-Metal Arc Welding 124,000 Thermal Plasma Chemical Vapor Deposition of Advanced Materials 157,975 Research on Combustion-Driven HVOF Thermal Sprays 96,893 Effect of Forced and Natural Convection on Solidification of Binary Mixtures 0 Materials Properties. Behavior. Characterization or Testing $ 2,579,682

Continuum Damage Mechanics - Critical States 0 An Investigation of History-Dependent Damage in Time-Dependent Fracture Mechanics 99,729 Intelligent Control of Thermal Processes 517,000 Elastic-Plastic Fracture Analysis Emphasis on Surface Flaws 132,000 Nondestructive Evaluation of Superconductors 205,000 Origins of Asymmetric Stress-Strain Response in Phase Transformations 80,535 Modeling and Analysis of Surface Cracks 192,000 Development of Measurement Capabilities for the Thermophysical Properties of Energy-Related Fluids 425,000 High-T¢ Superconductor-Semiconductor Integration and Contact Technology 116,800 Thin Film Characterization and Flaw Detection 0 Transport Properties of Disordered Porous Media From the Microstructure 116,959 Inelastic Constitutive Equation: Deformation Induced Anistropy and the Behavior at High Homologous Temperature 149,828 Stress and Stability Analysis of Surface Morphology of Elastic and Piezoelectric Materials 137,700 Optical Techniques for Characterization of High Temperature Superconductors 231,000 3-D Experimental Fracture Analysis at High Temperatures 76,721 Simulation and Analysis of Dynamic Failure in Ductile Materials 99,410

66 Office of Energy Research

OFFICE OF ENERGY RESEARCH (continued)

FY 1996

Office of Basic Energy Sciences (continued)

Division of Engineering and Geosciences (continued)

Engineering Sciences Research (continued)

Device or Component Fabrication. Behavior or Testing $ 357,423

An Analytical-Numerical Alternating Method for 3-D Inelastic Fracture and Integrity Analysis of Pressure-Vessels and Piping at Elevated Temperatures 85,000 Pulse Propagation in Inhomogeneous Optical Waveguides 200,493 Flux Flow, Pinning and Resistive Behavior in Superconducting Networks 71,930

Geosciences Research $2,957,219

Materials Preparation. Synthesis. Deposition. Growth or Forming $ 620,789

Organic Anion-Mineral Surface Interactions During Diagenesis 200,000 Solution-reprecipitation of Calcite and Partitioning of Divalent Metals 129,999 Transition Metal Catalysis in the Generation of Petroleum and Natural Gas 109,313 Mineral Dissolution and Precipitation Kinetics: A Combined Atomic-Scale and Macro-Scale Investigation 181,477

Materials Structure and Composition $ 519,258

Reaction Mechanisms of Clay Minerals and Organic Diagenesis: An HRTEM/AEM Study 139,065 Infrared Spectroscopy and Hydrogen Isotope Geochemistry of Hydrous Silicate Glasses 141,634 Biomineralization: Systematics of Organic-directed Controls on Carbonate Growth Morphologies and Kinetics Determined By in situ Atomic Force Microscopy 38,559 Reactions and Transport of Toxic Metals in Rock-Forming Silicates at 25°C 200,000 The Crystal Chemistry and Structural Analysis of Uranium Oxide Hydrates 0

Materials Properties. Behavior. Characterization or Testing $1,817,172 Oxygen and Cation Diffusion in Oxide Materials 180,000 Structure and Reactivity of Ferric Oxide and Oxyhydroxide Surfaces: Quantum Chemistry and Molecular Dynamics 200,000 Cation Diffusion Rates in Selected Silicate Minerals 150,000 Grain Boundary Transport and Related Processes in Natural Fine-Grained Aggregates 0 Thermodynamics of Minerals Stable Near the Earth's Surface 150,000 New Method for Determining Thermodynamic Properties of Carbonate Solid-Solution Minerals 133,661 Theoretical Studies of Metal Species in Solution and on Mineral Surfaces 55,817 Micromechanics of Failure in Brittle Geomaterials 223,820 Three-Dimensional Imaging of Drill Core Samples Using Synchrotron-Computed Microtomography 225,000 Shear Strain Localization and Fracture Evolution in Rocks 144,987 Dissolution rates and surface chemistry of feldspar glass and crystal 107,026 Transport Phenomena in Fluid-Bearing Rocks 0 Cation Chemisorption at Oxide Surfaces and Oxide-Water Interfaces: X-Ray Spectroscopic Studies and Modeling 246,861

67 Office of Energy Research

OFFICE OF ENERGY RESEARCH (continued)

FY 1996

Office of Computational and Technoloav Research $13,702,000

Division of Advanced Eneray Projects and Technoloay Research $13,702,000

Laboratory Technoloav Research (LTR) Proaram $ 8,062,000

Materials Preparation. Synthesis. Deposition. Growth or Forming $ 2,887,000

Lumeloid, A New Solar Energy Conversion Material (ANL94-42) 200,000 Cold Cathode Electron Emission from Diamond and Diamond-Like Carbon Thin Films for Flat Panel Computer Displays (ANL95-02) 140,000 Giant Magnetoresistance Wire Sensor (ANL95-07) 75,000 High Performance Tailored Materials for Levitation and Permanent Magnetic Technologies (ANL97-02) 125,000 Synthesis and Crystal Chemistry of Technologically Important Ceramic Membranes (ANL97-06) 125,000 Composite Metal-Hydrogen Electrodes for Metal-Hydrogen Batteries (BNL94-06) 115,000 Development of CdTe/CdZnTe Materials for Radiation Detectors (BNL94-09) 115,000 Corrosion Resistance of New Alloys for Biomedical Applications (BNL94-20) 140,000 Catalytic Production of Organic Chemicals Based on New Homogeneously Catalyzed Ionic Hydrogenation Technology (BNL97-05) 118,000 Novel Biocompatible 'Smart' Contact Lens Material (LBL94-28) 211,000 Alloy Design of Neodymium (Nd2 Fe,4 B) Permanent Magnets (ORL94-15) 155,000 Development of Aluminum Bridge Deck System (ORL94-56) 105,000 Manufacturing of Ni-Base Superalloys with Improved High-Temperature Performance (ORL95-05) 137,000 New Thermoelectric Materials for Solid State Refrigeration (ORL95-10) 150,000 Polymer Multilayer (PML) Film Applications of Optics, Electrolytes, and Glazings (PNL94-06) 200,000 Development of Mixed Metal Oxides (PNL94-28) 25,000 Development of Tape Calendaring Technology for Separation Membranes (PNL95-04) 257,000 Innovative Multilayer Thermal Barrier Coatings for Gas Turbine Engines (PNL95-07) 245,000 Interfacial Interactions of Biological Polymers with Model Surfaces (PNL97-21) 124,000 Highly Dispersed Solid Acid Catalysts on Mesoporous Silica (PNL97-28) 125,000

Device or Component Fabrication. Behavior or Testing $ 3,074,000

Application of High Performance Computing of Automotive Design and Manufacturing (ANL94-54) 175,000 Development of Rapid Prototyping Technology for Bioceramic Applications (ANL95-08) 276,000 Smooth Diamond Films for Friction and Wear Applications and Chemically Protective Coatings (ANL97-05) 150,000 Microfabrication of a Multi-Axis Micro-Accelerometer Using High Aspect Ratio Microfabrication (HARM) and Silicon Micromachining (BNL94-02) 100,000 Nondestructive X-Ray Scattering Characterization of High Temperature Superconducting Wires (BNL95-10) 160,000 Thin Film Lithium Batteries (BNL95-11) 80,000 New Catalysts for Direct Methanol Oxidation Fuel Cells (BNL95-14) 80,000 Development of Multi-Channel ASICs for CdZnTe Gamma Detectors Arrays (BNL97-06) 82,000 Microcircuits and Sensors for Portable, Low-Power Data Collection and Transmission (BNL97-07) 125,000

68 Office of Energy Research

OFFICE OF ENERGY RESEARCH (continued)

FY 1997

Office of Computational and Technoloya Research (continued)

Division of Advanced Eneray Proiects and Technoloav Research (continued)

Laboratory Technoloav Research Program (continued)

Device or Component Fabrication. Behavior or Testing (continued)

Rechargeable Zinc/Air Batteries for Consumer Applications (LBL94-43) 62,000 Micromagnetic Structures (LBL95-12) 378,000 Development of Zinc/Nickel Oxide Batteries for Electric Vehicle Applications (LBL95-27) 42,000 Catalytic Conversion of Chloro-Fluorocarbons Over Palladium-Carbon Catalysts (LBL95-45) 275,000 lonically Conductive Membranes for Oxygen Separation (LBL97-03) 125,000 Light Emission Processes and Dopants in Sold State Light Sources (LBL97-13) 125,000 Combinatorial Discovery and Optimization of Novel Materials for Advanced Electro-Optical Devices (LBL97-18) 125,000 Development of a Thin-Film Battery Powered Hazard Card and Other Microelectronic Devices (ORL94-39) 74,000 Ion Implantation Processing Technologies (ORL94-72) 136,000 Rapid Prototyping of Ceramics (ORL94-95) 153,000 Development of a Thin Film Battery Powered Transdermal Medical Device (ORL95-11) 187,000 Rapid Prototyping of Bioceramics for Implants (ORL95-12) 64,000 Development of High-Temperature Superconducting Wire Using RABITS Coated Conductor Technologies (ORL97-02) 100,000

Instrumentation and Facilities $ 1,079,000

Micro-Spectroscopy Facility for New Infrared Imaging Materials (BNL94-60) 91,000 Development of Environmentally Conscious Machining Fluids (ORL94-91) 204,000 Novel Methods for Fabrication Cost Reduction of Pressure Infiltration Cast Metal Matrix Composite Components (ORL95-01) 192,000 Ultra-Precision Automated Measurement for Manufacturing (ORL95-08) 75,000 Neural Network Model (ORL95-90) 248,000 Microfabricated Instrumentation for Chemical Sensing in Industrial Process Control (ORL97-08) 99,000 Modeling and Simulation of Advanced Sheet Metal Forming (PNL94-38) 170,000

Materials Properties. Behavior. Characterization of Testing $1,022,000

Next Generation Corrosion Inhibitors for Steel in Concrete (BNL95-12) 50,000 Prevention/Elimination of Metal-Water Explosions in Aluminum Casting Pits (ORL92-05) 174,000 In-Line Aluminum Sensors (ORL95-04) 113,000 The Role of Yttrium in Improving the Oxidation Resistance in Advanced Single Crystal Nickel-based Superalloys for Turbine Applications (ORL95-07) 149,000 Atomic Scale Structure of Ultrathin Magnetic Multilayers and Correlation with Resistance, Giant Magnetoresistance, and Spin-Dependent Tunneling (ORL97-03) 100,000 Processing/Property Relationships in Centrifugally Cast Al-Metal Matrix Composites (MMC) (PNL94-02) 245.000 Bioactive and Porous Metal Coatings for Improved Tissue Regeneration (PNL95-23) 191,000

69 Office of Energy Research

OFFICE OF ENERGY RESEARCH (continued)

FY 1997

Office of Computational and Technology Research (continued)

Division of Advanced Eneray Proiects and Technoloav Research (continued)

Advanced Energy Projects Program $5,640,000

Device or Component Fabrication. Behavior or Testing $2,553,000

Composite Magnetostrictive Materials for Advanced Automotive Magnetomechanical Sensors 449,000 Energy Related Applications of Selective Line Emitters 266,000 Investigation of High Efficiency Multi Band Gap Multiple Quantum Well Solar Cells 225,000 A Novel Tandem Homojunction Solar Cell: An Advanced Technology for High Efficiency Photovoltaics 255,000 Magnetically Enhanced Thermoelectric Cooling 250,000 Photochemical Solar Cells 150,000 Efficient Energy Up-Conversion of Infrared to Visible Light at Semiconductor Heterojunctions 268,000 Electrically Active Liquid Matrix Composites 300,000 Semiconductor Broadband Light Emitters 390,000 Materials Preparation. Synthesis. Deposition. Growth or Forming $2,178,000

Next Generation High-Temperature Structural Materials for Heat Exchangers and Heating Elements 294,000 Photorefractive Liquid Crystals: New Materials for Energy-Efficiency Imaging Technology 289,000 Tritiated Porous Silicon: A Standalone Power Source 250,000 Supported Molten Metal Catalysts: Development of a New Class of Catalysts 322,000 Combinatorial Synthesis of High Tc Superconductors 250,000 Fabrication and Characterization of Micron Scale Ferromagnetic Features 106,000 Micro-Hollow Cathode Discharge Arrays: High Pressure, Nonthermal Plasma Sources 259,000 Rapid Melt and Resolidification of Surface Layers Using Intense, Pulsed Ion Beams 300,000 Experimental and Theoretical Investigation of Dual-Laser Ablation for Stiochiometric Large-Area Multicomponent Film Growth 108,000

Materials Properties. Behavior. Characterization or Testing $ 909,000

Shape Memory Alloy Reinforcement of Metals 405,000 Exploitation of Room Temperature Molecule/Polymer Magnets for Magnetic and Electromagnetic Interference Shielding and Electromagnetic Induction Applications 212,000 Molecular Surface Modification as a Means of Corrosion Control 292,000

70 Office of Energy Research

OFFICE OF ENERGY RESEARCH (continued)

FY 1997

Office of Computational and Technoloyv Research (continued)

Division of Advanced Eneray Projects and Technology Research (continued)

Small Business Innovation Research Proaram $58,849,611

Materials. Preparation. Synthesis. Deposition. Growth or Forming $17,920,148

Phase I $3,368,833

Controlled Permeability Chemically Activated Fly Ash (CAFA) for Reactive Contaminant Barrier 75,000 Advanced Multilayer Braze Foil for Si3N4 Joining 74,997 A Novel Reactive Joining Compound for High Temperature Applications 74,993 Fabrication of Active Braze Alloys for High Temperature Service 75,000 Diamond-Like Nanocomposites: Hard, Wear Resistant, Low Friction Coatings for Tribological Applications 74,869 High Growth Rate Cubic Boron Nitride Deposition 74,867 Development of Novel Boron-Based Multilayer Thin-Film 73,420 Nano-Layered Diboride Materials with Enhanced Hardness, Strength, and Toughness for Wear Applications 74,929 Advanced Plasma Surface Modification System 74,669 High-Flux, Low Energy, Ion Source for High Rate Ion-Assisted Deposition of Hard Coatings 75,000 An Ion Source Design Useful for the Production of Tribiological Thin Films 74,996 Semi-Solid Thermal Transformation to Produce Semi-Solid Formable Alloys 75,000 A Simple Process to Manufacture Grain Aligned Permanent Magnets 74,840 A Novel Technique for the Enhancement of Coercivity in High Energy Permanent Magnets 73,130 Controlled Atmosphere Plasma Spraying of NdFeB Magnet Materials 75,000 Stabilization of Nitride Magnet Material Via Sol-Gel Route 75,000 A Novel Process to Produce Nanostructured Permanent Magnetic Materials 75,000 Coke Resistant Catalyst for the Partial Oxidation Reforming of Hydrocarbon Fuels 75,000 CO Tolerant Doped-Metal Oxide Catalysts 74,987 Advanced Electrocatalysts for Direct Methanol Oxidation 74,974 A Combinatorial Approach to the Synthesis and Characterization of Novel Anode Materials for Direct Methanol Fuel Cells 74,582 Novel Multifunctional Direct Methanol Fuel Cell Catalysts 75,000 Low Cost Deposition of Buffer Layers for Manufacturable YBCO HTS Conductors 75,000 Stoichiometric YBCO Epitaxial Coatings on RABITS Using Low Cost CCVD Processing 75,000 Buffer Layers on Textured Nickel Using Commercially Viable CCVD Processing 75,000 Micromachined SiC Sensors For Harsh Environment Applications 75,000 Silicon Carbide Sensors for Harsh Environments 74,840 Development of Efficient and Practical Passive Solar Building Systems with High Recycled Content Using the Preplaced Aggregate Concrete Technology 75,000 Heterogeneous Hydroformylation of Alkanes with Syngas 75,000 Advanced NZP-Ceramic Based Thermal Barrier Coatings with Enhanced Oxidation and Thermal Shock Resistance 74,900

71 Office of Energy Research

OFFICE OF ENERGY RESEARCH (continued)

FY 1997

Office of Computational and Technology Research (continued)

Division of Advanced Energy Projects and Technology Research (continued)

Small Business Innovation Research Program (continued)

Materials. Preparation. Synthesis. Deposition. Growth or Forming (continued)

Phase I (continued)

Tubular SOFC with Deposited Nano-Scale YSZ Electrolyte 75,000 Integrated Bandpass Filter Contacts for TPV Cells 74,976 In-Situ Ultrahigh-Pressure Waterjet Peening of Nuclear Reactor Internals for the Prevention of Stress Corrosion Cracking 74,879 Thallium-Containing Ill-V Quaternary Compound Semiconductor for Use in Infrared Detection 75,000 High Speed Long Wavelength Infrared Detector Array/Preamplifier Development 75,000 Development of Cadmium Germanium Arsenide Crystals 74,995 AlInGaN Light Emitting Diodes for Spectroscopic Applications 74,195 An Easily Dispersed Reactive Coating for Surface Decontamination 75,000 High Quantum Efficiency Spin-polarized Photocathodes 74,991 Rapid Quench Nb3AI for High Field Accelerator Applications 75,000 Ultra-Lightweight Carbon-Carbon Cooling Structure For Pixel and Silicon Strip Detectors 75,000 Epitaxial Growth of SiC on Silicon for Radiation Hard Particle Detectors 74,873 Development of Scintillators and Waveshifters for Detection of Ionizing Radiation 75,000 Low Viscosity Organic Insulation Systems For Improved Processing and Reduced Radiation Induced Gas Evolution 74,994 Radiation Resistant Joining Methods for Structural Applications in Fusion Energy Systems 74,937

Phase II (First Year) $5,802, 195

An Attrition-Resistant Zinc Titante Sorbent for a Transport Reactor 750,000 A Light Scattering Based Sensor for On-Line Monitoring of Fiber Diameter Distribution During Fiberglass Manufacturing 561,744 Novel Use of Gas Jet Plasma to Prepare Amorphous Silicon Alloy 750,000 High Rate Deposition of Transparent Conducting Zinc Oxide Using Activated Oxygen for Photovoltaic Manufacturing Cost Reduction 744,962 Development of Optimal SnO2 Contacts for CdTe Photovoltaic Applications 750,000 Large Area, Low Cost Processing for CIS Photovoltaics 750,000 Improved Processes for Forming CIS Films 750,000 Ultrafast Polysilylene Scintillators 745,489

72 Office of Energy Research

OFFICE OF ENERGY RESEARCH (continued)

FY 1997

Office of Computational and Technoloav Research (continued)

Division of Advanced Enerav Proiects and Technoloav Research (continued)

Small Business Innovation Research Program (continued)

Materials. Preparation. Synthesis. Deposition. Growth or Forming (continued)

Phase II (Second Year)

Low Cost, Contamination-Tolerant Electrocatalysts for Low-Temperature Fuel Cells 750,000 A Low Cost, High Temperature Superconductor Wire Manufacturing Technology 750,000 A Low Cost Receiver Plate Manufacturing Process for High Concentration Photovoltaic Systems 680,000 An Intumescent Mat Material for Joining of Ceramics to Metals at High Temperatures 750,000 Development of Modulator Quality Rubidium Titanyl Arsenate Crystals for Remote Sensing Laser Systems 750,000 A Novel Method to Recycle Thin Film Semiconductor Materials 600,000 An Improved Material and Low-Cost Fabrication Options for Candle Filters 750,000 An Integrated Catalyst/Collector Structure for Regenerative Proton-Exchange Membrane Fuel Cells 719,147 Nanostructured Interstitial Alloys as Catalysts for Direct Energy Applications 750,000 Environmentally Responsible Recycling of Thin-Film Cadmium Telluride Modules 750,000 Low-Cost, Large-Area, High-Resistivity Substrates for Gas Microstrip Detectors 749,973 An Economic Sorbent for the Removal of Mercury, Chlorine, and Hydrogen Chloride from Coal Combustion Flue Gases 750,000

Materials ProDerties. Behavior. Characterization or Testing $12,202,888

Phase I $ 971,422

Nondestructive Measurements of Key Mechanical Properties of Alloy 718 Welded Structures Using Novel Stress-Strain Microprobe Technology 75,000 Processing For Surface Hardness: Novel Characterization Techniques for Dynamic Tribological Properties of Thin Films 74,993 A Novel Mass Spectrometer for Characterization of Electrochemical Processes 75,000 New Insulation Techniques for High Voltage, High Frequency Motors 74,985 Development of Carbon Products from the Waste Stream of the Super Critical Deashing Process in Coal Liquefaction 75,000 Sol-Gel Coatings as Corrosion Barriers for Carbonate Fuel Cell Components 75,000 Enhanced Flaw Detection by Time-Reversal Auto-Focusing of an Ultrasonic Array 74,988 High Resolution Cryogenic Calorimeter for Beta and Gamma Ray Detection 74,976 High Current Density High Repetition Rate Ferroelectric Cathode 75,000 High Current Capacity High Temperature Superconducting Film Based Tape for High Field Magnets 75,000 A Polycrystalline Pixel Diamond Film Particle Detector 71,483 Resistance Welding Vanadium Alloys 74,997 Low Cost Technique for Testing Ceramic Insulator Coatings 75,000

73 Office of Energy Research

OFFICE OF ENERGY RESEARCH (continued)

FY 1997

Office of Computational and Technoloav Research (continued)

Division of Advanced Eneray Proiects and Technoloav Research (continued)

Small Business Innovation Research Program (continued)

Materials Properties. Behavior. Characterization or Testing (continued)

Phase II (First Year) $8,242,295

Carbon Monoxide Tolerant Anodes for Proton Exchange Membrane (PEM) Fuel Cells 750,000 Low Cost Advanced Bipolar Plates for Proton Exchange Membrane Fuel Cells 720,000 Improved Bi-2223 Flux Pinning Through Chemical Doping 750,000 Low Cost Multifilament Composite Process 750,000 Template-Mediated Synthesis of Periodic Membranes for Improved Liquid-Phase Separations 750,000 Novel Fiber-Based Adsorbent Technology 750,000 Metal-Binding Silica Materials for Wastewater Cleanup 750,000 Superhard Nanophase Cutter Materials for Rock Drilling Applications 750,000 Evaluation and Constitutive Modeling of Unidirectional SiC/SiC Composites with Engineered SiC Fiber Coatings Subjected to Neutron Irradiation 748,520 Innovative Fabrication of SiC/SiC Composites with High Through-the- Thickness Thermal Conductivity 750,000 High Numerical Aperture Scintillating Fibers 743,775

Phase II (Second Year) $2,989,171

Rotating, In-Plane Magnetization and Magneto-Optic Imaging of Cracks Under Coatings on Ferromagnetic Metals 750,000 Development of Laser Materials and Rugged Coatings as Components for Tunable Ultraviolet Laser Systems 739,171 Application of Raman Spectroscopy to Identification and Sorting of Post-Consumer Plastics for Recycling 750,000 A Sensor for Automated Plastics Sorting 750,000

Device or Component Fabrication. Behavior or Testing $28,726,575

Phase I $ 2,095,557

Hydrocarbon Gas Sensors Based on Wide Band-Gap Semiconductors 74,195 Shaft Weld Replacement with a Ceramic Locking Assembly Joint 74,986 A Novel Technology for Si3N4-To Superalloy Joints With High Use Temperature Capability 75,000 Development of Economical Procedures for Producing and Processing Fine Grained SSM Feedstock via Mechanical Stirring 72,667 A New Semi-Solid Forming Process For Fabrication of High Volume Fraction (>15 vol%) Metal/Metal Carbide Nanocomposites 75,000 Alternative Metal Forming Using Laser Engineered Net Shaping 74,777 Production of High Performance BSCCO-2223 Tapes Using Hydrostatic Pressure 75,000 Development of Long-length Fabrication Technology for High Tc Superconductors Operation in High Magnetic Fields at 77K 74,999

74 Office of Energy Research

OFFICE OF ENERGY RESEARCH (continued)

FY 1997

Office of Computational and Technoloav Research (continued)

Division of Advanced Eneray Projects and Technoloov Research (continued)

Small Business Innovation Research Program (continued)

Device or Component Fabrication. Behavior or Testing (continued)

Phase I (continued)

Non-Linear Inductor for Power Electronics Protection 75,000 Novel Fabrication of Low Cost Performance Bipolar Plates 75,000 Corrosion Resistant Bipolar Plates for PEM Fuel Cells 74,989 Reduced Part Count Motor Fabrication 74,900 Removal of Particulate and SO/NO, Precursors in Integrated Gasification Combined Cycle Systems 75,000 Use of Novel, Low-Cost Additives to Improve Sorbent Efficiency for Control of Mercury Emissions in Coal-Fired Power Plant Flue Gases 74,996 Mixed Phase Positive Electrodes for Long Life AMTEC Modules 75,000 High Brightness LEDs Based on the (AI,Ga,ln)N Materials System 75,000 Development of High Power RF Windows and Waveguide Components for the Next Linear Collider 75,000 Cost Reduction for Production of Superconducting Niobium Cavities 74,355 Electrical Discharge Machining Application to the Development of mm-wave Accelerating Structures 74,000 Direct Adhesive Technology for Arbitrary Conductors 74,839 Controlled Processing for High-Performance Fine Filament Bi-2223 Conductors 75,000 Development of a High Field NbTi Superconductor Using an Approach Combining Artificial Flux Pinning With Conventional Thermomechanical Processing 74,993 Conventionally Processed NbTi Superconductors with Artificial Ferromagnetic Pinning Centers for High Magnetic Field (>8 T) Application 74,997 Liquid Core Optical Scintillating Fibers 74,973 High Performance Heat Pipe Cooling of Electron Cyclotron Heating Mirrors P12-2426 74,971 Reaction Bonding of Silicon Carbide Composites for Fusion Applications 74,945 Net Shape Gradient W-Cu Plasma Facing Components by Pressure Infiltration 74,975 Joining of Silicon Carbide for Fusion Applications 75,000 A Novel Divertor Design Based on a Tungsten Wire Brush Tile 75,000 Beryllium and Tungsten Brush Armor for Plasma Facing Components 75,000 Fabrication for Reliable Tungsten Brush Structures for Fusion Reactor Applications 75,000

Phase II (First Year) $20,090,139

Catalytic Membrane for High Temperature Hydrogen Separations 750,000 Advanced Coal Based Power System'Components Using Reaction Bonded Silicon Carbide 749,449 A New Separation and Treatment Method for Soil and Groundwater Restoration 749,529 Continuous Analyzer for Monitoring Hydrogen Chloride and Chlorine During Site Cleanup Activity 749,701 Long-Life Electrical Neutron Generator 750,000 Passive Electronic Components from Nanostructured Materials 750,000 A Multicore Optical Fiber Sensor for Mass Transport and Particulates 749,991 Infrared Hollow Waveguide Organic Solvent Analyzer 749,929

75 Office of Energy Research

OFFICE OF ENERGY RESEARCH (continued)

FY 1997

Office of Computational and Technology Research (continued)

Division of Advanced Enerav Projects and Technoloav Research (continued)

Small Business Innovation Research Program (continued)

Device or Component Fabrication. Behavior or Testing (continued)

Phase II (First Year) (continued)

Stratospheric Water Vapor Microsensor 750,000 Compact, Airborne Laser Multigas Sensor 600,443 Microwave Radiometer for Passively and Remotely Measuring Atmospheric Water Vapor 738,746 Advanced Water Sensor for Unmanned Aerial Vehicles 750,000 High-Gain Monocapillary Optics 539,595 High Performance X-Ray and Neutron Microfocusing Optics 517,510 Very Low Friction Small Radius Domed Cutters for Percussion Drill Bits 750,000 Development and Testing of a Jet Assisted Polycrystalline Diamond Drilling Bit 750,000 Advanced Low-Stress Bonding of Thermally Stable Polycrystalline Diamond Cutters to Tungsten Carbide Substrates 749,968 Nanocrystalline Superhard, Ductile Ceramic Coatings for Roller Cone Bit Bearings 749,707 Solid-State Ultracapacitors for Electric Vehicles and Consumer Electronics 750,000 High Surface Area Non-Oxide Ceramic Electrodes for Ultracapacitors 750,000 Wrappable Inorganic Electrical Insulators for Superconducting Magnets 750,000 Joining of Tungsten Armor Using Functional Gradients 750,000 Carbon Thermostructure for Silicon-Based Particle Detectors 750,000 High Performance Optical Detectors for Calorimetry 750,000 Coplanar CdZnTe p-l-n, Gamma-Ray Detectors for Nuclear Spectroscopy 745,571 Large Room Temperature CdxZnxT, Detectors 750,000 In-Situ Nondestructive Measurements of Key Mechanical Properties of Reactor Pressure Vessels Using Innovative SSM Technology 600,000 Oxidation Induction Time Technology for Electric Cable Condition Monitoring and Life-Assessment 600,000

Phase II (Second Year) $6,540,879

Advanced High Power Silicon Carbide Internally Cooled X-Ray 749,291 Chemical Microsensor Arrays as Integrated Chip Compatible Devices for Chemical Weapons Nonproliferation Inspection 600,787 A High Resolution Multi-hit Time to Digital Converter Integrated Circuit 749,890 A Helium-Cooled Faraday Shield Using Porous Metal Cooling 695,343 Low Cost Fabrication of Large Silicon Carbide/Silicon Carbide Composite Structures 750,000 Bandgap-Engineered Thermophotovoltaic Devices for High Efficiency Radioisotope Power 747,791 Rugged, Tunable Infrared Laser Sources 750,000 An Innovative Membrane and Process for Removal and Recovery of Natural Gas Liquids 750,000 A Lower Cost Molten Carbonate Matrix 747,777

76 Office of Energy Research

OFFICE OF ENERGY RESEARCH (continued)

FY 1997

Office of Computational and Technoloav Research (continued)

Division of Advanced Energy Projects and Technologv Research (continued)

Small Business Technoloav Transfer Program $4,099,589

Materials Preparation. Synthesis. Deposition. Growth or Forming $2,299,868

Phase I $ 299,891

Improved Beta-Alumina Fabrication Using Rapid Plasma Sintering 99,896 New High-Performance GaSb-Based Thermophotovoltaic (TPV) Devices 99,995 High Efficiency Magnet Refrigerators as Alternate Environmentally Safe Commercial Refrigeration Devices 100,000

Phase II (First Year) $ 499,977

Cabled Monofilament Subelements for Improved Multifilament Niobium Tin Performance and Reduced Cost 499,977

Phase II (Second Year) $1,500,000

Laser Processing of Thermal Sprayed Beryllium Plasma Facing Components 500,000 Amorphous Silicon/Crystalline Silicon Heterojunctions for Nuclear Radiation Detector Applications 500,000 Low Loss Sapphire Windows for High Power Microwave Transmission 500,000

Device or Component Fabrication. Behavior or Testing $1,799,721

Phase I $ 299,761

Novel Thin Film Scintillator for Intermediate Energy Photons Detection and Imaging 99,796 Silicon Carbide Heat Exchanger for Advanced Coal-Based Power Systems 99,965 Advanced Ceramic Hot Gas Filters 100,000 Phase II (First Year) $ 999,960

High Speed Motor Alternators for Hybrid Electric Vehicle Energy Storage 499,960 A Flywheel Motor Alternator for Hybrid Electric Vehicles 500,000

Phase II (Second Year) $ 500,000

Environmentally Benign Manufacturing of Compact Disk Stampers 500,000

77 Office of Energy Research

OFFICE OF ENERGY RESEARCH (continued)

FY 1997

Office of Fusion Enerav Sciences $11,178,000

Materials Properties. Behavior. Characterization or Testing $11,178,000

Structural Materials Development 670,000 Modeling Irradiation Effects in Solids 50,000 Fusion Systems Materials 3,270,000 Structural Materials for Fusion Systems 960,000 Development of Radiation-hardened Ceramic Composites for Fusion Applications 28,000 Damage Analysis And Fundamental Studies for Fusion Reactor Materials Development 150,000 Development of Lithium-bearing Ceramic Materials for Tritium Breeding in Fusion Reactors 100,000 Post-irradiation Examination of Lithium-bearing Ceramic Materials for Tritium Breeding in Fusion Reactors 20,000 International Thermonuclear Experimental Reactor (Iter) Materials Development for Plasma Facing Components 5,000,000 ITER Materials Evaluation 330,000 ITER Structural Materials Evaluation 200,000 Development of Nb3sn Superconducting Wire for the ITER Magnet Program 200,000 Structural Materials Development for the Conduit of ITER Cable-in-Conduit-Conductors 200,000

78 Office of Energy Research

OFFICE OF ENERGY RESEARCH

The Office of Energy Research (ER) advances the science and technology foundation for the Department and the Nation to achieve efficiency in energy use, diverse and reliable energy sources, a productive and competitive economy, improved health and environmental quality, and a fundamental understanding of matter and energy. The Director of Energy Research is responsible for six major outlay programs: Basic Energy Sciences, Fusion Energy, Health and Environmental Research, High Energy and Nuclear Physics and Computational and Technology Research. The Director also advises the Secretary on DOE physical research programs, university-based education and training activities, grants, and other forms of financial assistance.

The Office of Energy Research conducts materials research in the following offices and divisions:

* Office of Basic Energy Sciences - Division of Engineering and Geosciences; Division of Materials Sciences; and Division of Chemical Sciences

* Office of Computational and Technology Research - Division of Advanced Energy Projects and Technology Research

Office of Health and Environmental Research - Division of Physical and Technology Research

Office of Fusion Energy - Division of Advanced Physics and Technology

Materials research is carried out through the DOE national laboratories, other federal laboratories, and grants to universities and industry.

OFFICE OF BASIC ENERGY SCIENCES

The Office of Basic Energy Sciences (BES) supports basic research in the natural sciences leading to new and improved energy technologies and to understanding and mitigating the environmental impacts of energy technologies. The BES program is one of the Nation's foremost sponsors of fundamental research in broad areas of materials sciences, chemical sciences, geosciences, biosciences, and engineering sciences. The BES program underpins the DOE missions in energy and the environment, advances energy-related basic science on a broad front, and provides unique national user facilities for the scientific community.

The program supports two distinct but interrelated activities: (1) research operations, primarily at U.S. universities and 11 DOE national laboratories and (2) user-facility operations, design, and construction. Encompassing more than 2,400 researchers in 200 institutions and 17 of the Nation's premier user facilities, the program involves extensive interactions at the interagency, national, and international levels. All research activities supported by BES undergo rigorous peer evaluation through competitive grant proposals, program reviews, and advisory panels. The challenge of the BES program is to simultaneously achieve excellence in basic research with high relevance to the Nation's energy future, while providing strong stewardship of the Nation's research performers and the institutions that house them to ensure stable, essential research communities and premier national user facilities.

DIVISION OF MATERIALS SCIENCES

The Division of Materials Sciences conducts a broad program of materials research to increase the understanding of phenomena and properties important to materials behavior that will contribute to meeting the needs of present and future energy technologies. The Division supports fundamental research in materials at DOE national laboratories and plans, constructs, and operates national scientific user facilities needed for materials research. In addition, the Division funds over 200 grants, mostly with universities, on a wide range of topics in materials research.

Fundamental materials research is carried out at twelve DOE laboratories: Ames Laboratory at Iowa State University, Argonne National Laboratory, Brookhaven National Laboratory, Idaho National Engineering Laboratory, Lawrence Berkeley National Laboratory, Los Alamos National Laboratory, National Renewable Energy Laboratory, Oak Ridge National Laboratory, Pacific Northwest National Laboratory, and Sandia National Laboratories in New Mexico and California, and the Stanford Synchrotron Radiation Laboratory. The laboratories also conduct significant research

79 Office of Energy Research activities for other DOE programs such as Energy Efficiency, Fossil Energy, Nuclear Energy, Environmental Management and Defense Programs. The Division of Materials Sciences also funds a program consisting of 50 research projects at the University of Illinois Frederick Seitz Materials Research Laboratory.

The performance parameters, economics, environmental acceptability and safety of all energy generation, conversion, transmission, and conservation technologies are limited by the discovery and optimization of the behavior and performance of materials in these energy technologies. Fundamental materials research seeks to understand the synergistic relationship between the synthesis, processing, structure, properties, behavior, performance of materials of importance to energy technology applications and recycling of materials. Such understanding is necessary in order to develop the cost-effective capability to discover technological and economically desirable new materials and cost- competitive and environmentally acceptable methods for their synthesis, processing, fabrication, quality manufacture and recycling. The materials program supports strategically relevant basic scientific research that is necessary to discover new materials and processes and to eventually find optimal synthesis, processing, fabricating, and manufacturing parameters for materials. Materials Science research enables sustainable development so that economic growth can be achieved while improving environmental quality.

Specific information on the Materials Sciences sub-program is contained in the DOE publication DOE/ER-0703 Materials Sciences Programs FY 1996 (published June 1997). This 168-page publication contains program descriptions for 478 research programs that were funded in Fiscal Year 1996 by the Division of Materials Sciences. Five cross-cutting indices identify all 478 programs according to Principal Investigator(s), Materials, Techniques, Phenomena and Environment. Other contents include identification of the Division of Materials Sciences Staff structure and expertise; a bibliographical listing of 48 scientific workshop, topical, descriptive, Research Assistance Task Force and research facilities reports on select topics that identify materials sciences research needs and opportunities; a descriptive summary of the DOE Center of Excellence for the Synthesis and Processing of Advanced Materials; a descriptive summary and access information on 15 National Research User Facilities including synchrotron light sources, neutron beam sources, electron beam microcharacterization instruments, materials preparation and combustion research; and an analytical summary of research funding levels. Limited copies may be obtained by calling (301) 903-3427 and requesting DOE publication DOE/ER-0703. Project summaries are also available under the Division's home page on the Worldwide Web (www.er.doe.gov/production/ bes/dms/portfolio.html).

NATIONAL USER FACILITIES UNDER THE OFFICE OF BASIC ENERGY SCIENCES

Basic Energy Sciences (BES) is responsible for the planning, construction, and operation of many of the Nation's most sophisticated research facilities, including third-generation synchrotron light sources and high-flux neutron sources as well as specialized facilities for microcharacterization, materials synthesis and processing, combustion research, and ion beam studies. These facilities are unmatched in the world in their breadth of capabilities and number of scientific users. BES facilities have enormous impact on science and technology, ranging from the structure of superconductors and biological molecules to the development of wear-resistant prostheses, from atomic-scale characterization of environmental samples to elucidation of geological processes, and from the production of unique isotopes for defense applications and cancer therapy to the development of new medical imaging technologies.

BES research facilities serve over 4,500 researchers from universities, industry, and government laboratories each year. These users conducted forefront research in physics, materials sciences, chemical sciences, earth sciences, structural biology, engineering, medical and other sciences. The costs for the construction and the safe, user-friendly operation of these world class facilities are substantially beyond the capability of individual academic and private industrial research laboratories. They are made available to all qualified users from academia, industry, and both DOE and non-DOE government laboratories, most generally without charge for non-proprietary research that will be published in the open literature.

The research facilities permit the Nation's science and technology enterprise to have access to research instruments that are required for world-competitive forefront research that would not otherwise be possible. Included amongst the numerous honors and distinctions to the research that has been carried out at the BES national user facilities was the 1994 Nobel Prize in Physics, shared by Dr. Clifford G. Shull, who carried out pioneering investigations in neutron scattering at Oak Ridge National Laboratory. All of the BES national user facilities have been constructed within cost, on schedule, and with rigorous compliance to all environmental, safety and health regulations. Further information about the National User Facilities can be found in "Scientific Research Facilities," published by the U.S. Department of Energy; available from the Office of Basic Energy Sciences, (301) 903-3081.

80 Office of Energy Research

DIVISION OF CHEMICAL SCIENCES

The Division of Chemical Sciences supports research important to fossil chemistry, combustion, advanced fusion concepts, photoconversion, catalysis, separations chemistry, actinide and lanthanide chemistry, thermophysical properties of complex fluids, nuclear waste processing, and environmental remediation. Research related to materials is carried out in the areas of heterogeneous catalysis, electrochemical energy storage and conversion research and materials precursor chemistry. The operating budget for FY 1997 for materials-related programs was $5,143,000 and was allocated to 23 projects in heterogeneous catalysis, electrochemical energy storage and conversion research and materials precursor chemistry.

The program in catalysis emphasizes fundamental chemical, physical, materials and engineering aspects related to catalytic chemistry. Research into fundamental aspects of heterogeneous catalysis overlaps in several areas with complementary efforts in the Division of Materials Sciences. Among these areas are the synthesis of oxides having large surface areas and large pore volumes, but fairly small pores. This includes single and mixed oxides which are either crystalline or amorphous. Another area of overlap is the characterization of thin oxide films on metals. These materials not only have important relationships to industrial catalysts but also are intrinsically interesting and allow the types of detailed studies of ceramic type properties normally associated with single crystals. Structural studies on bimetallic crystals as model catalysts constitutes a second area of overlap. This area is closely tied to alloy physics. Finally, the reactive decomposition chemistry of chlorocarbons on single crystals has a strong relationship to corrosion and lubrication.

The Chemical Engineering Science program supports fundamental research in electrochemical energy storage and conversion focused on the non-automotive consumer market with emphasis on improvements in battery size, weight, life and recharge cycles. Areas of research include materials development and characterization, battery component development and interactions, characterizatioon methodologies and systems development and modeling. Although both primary and secondary battery systems are considered, the greatest emphasis is placed on rechargeable (i.e., secondary) battery systems. The program covers a broad spectrum of research including investigations of lithium cells, metal hydrides, fundamental studies of composite electrode structures, failure and degradation of active electrode materials, thin-film electrodes, electrolytes and interfaces. Characterization and methodologies include problems of electrode morphology, corrosion, separator/electrolyte stability, stable microelectrodes and the transport properties of electrode and electrolyte materials and surface films. Investigations in computational chemistry, modeling and simulations, including property predictions, phenomenological studies of reactions and interactions at critical interfaces, film formation, phase change effects on electrodes and characterization of crystalline and amorphous materials are also of interest.

Chemical Sciences-supported materials precursor chemistry centers on the chemistry of advanced materials precursors, including the synthesis of novel inorganic and organometallic and polymeric structures which could serve as precursors to ceramics and other advanced materials. The research is represented by the following areas: catalysis to link monomeric/polymer building blocks; the mechanisms of oligomerization steps; electronic theories to predict precursors for new ceramics; emerging advanced materials based on complex oxides; single source precursors to multicomponent oxides; the design of materials with tailored properties; and the synthesis and characterization of complex 3-dimensional structures.

The Division of Chemical Sciences manages several large scientific facilities. Four of these are user-oriented: the Combustion Research Facility at Sandia/California, the High Flux Isotope Reactor at Oak Ridge National Laboratory, the Stanford Synchrotron Radiation Laboratory at Stanford University and the National Synchrotron Light Source at Brookhaven National Laboratory. The National Synchrotron Light Source is operated in conjunction with the Division of Materials Sciences.

For information about specific programs the DOE contact is William S. Millman, (301) 903-3285. The reader also is referred to the Worldwide Web for the publication Summaries of FY 1997 Research in the Chemical Sciences (www.er.doe.gov/production/bes/chmhome.html) for summaries of all funded programs and descriptions of major user and other special facilities.

81 Office of Energy Research

DIVISION OF ENGINEERING AND GEOSCIENCES

Materials research in the Division of Engineering and Geosciences is sponsored by two different programs as described below.

The BES Engineering Research Program was started in 1979 to help resolve the numerous serious engineering issues impeding efforts to meet U.S. long-term energy needs. The program supports fundamental research on broad, generic topics in energy related engineering-topics not as narrowly scoped as those addressed by the shorter term engineering research projects sponsored by the various DOE technology programs. Special emphasis is placed on projects which, if successfully concluded, will benefit more than one energy technology.

The broad goals of the BES Engineering Research Program are: (1) to extend the body of knowledge underlying the current engineering practice so as to create new options for enhancing energy savings and production, for prolonging useful equipment life, and for reducing costs without degradation of industrial production and performance quality; and (2) to broaden the technical and conceptual base for solving future engineering problems in the energy technologies. The DOE contact for this program is Robert E. Price, (301) 903-5822.

ENGINEERING SCIENCES RESEARCH topics share some common features and physics which make it efficient and cost-effective to consider them A brief description of Engineering Sciences supported together. They forma a natural progression and will be programs is found in DOE/ER-0704, 'Summaries of pursued sequentially in the above order, but with FY 1996 Engineering Research," which was published significant overlap. in June 1997. Limited copies may be obtained by calling (301) 903-5822. Keywords: Plasma Processing, Functionally Gradient Materials MATERIALS PREPARATION, SYNTHESIS, DEPOSITION, GROWTH OR FORMING 164. MULTIVARIABLE CONTROL OF THE GAS- METAL ARC WELDING PROCESS 163. FUNDAMENTALS OF THERMAL PLASMA $153,000 PROCESSING DOE Contact: Robert E. Price, (301) 903-5822 $478,000 MIT Contact: David E. Hardt, (617) 253-2429 DOE Contact: Robert E. Price, (301) 903-5822 Idaho National Engineering Laboratory Continuing from last year we have been pursuing three Contact: J. R. Fincke, (208) 526-2031 related topics: development of a unique high bandwidth are-furnace, development of a 'variable footprint' This project is the experimental portion of a coordinated welding torch, and exploration of distributed parameter experimental-theoretical research project on thermal models, sensors and controllers. These topics are all plasma processing of materials. This work is primarily motivated by the need to have greater control over the focused on the development of advanced diagnostic spatial distributions, owing to the limitations imposed by and computational techniques and their application to a lumped parameter modeling approach. The arc obtain a better and more detailed understanding of the furnace work was completed this year, with demop- fundamental physical and chemical processes occurring stration of de-coupled temperature and flowrate control. in nonequilibrium thermal plasmas with entrained A U.S. patent has been issued for this furnace concept particles. The techniques thus developed and the infor- and the attendant control system. mation and insights they provide, can then be directly applied to process design, optimization, and scale-up. The work on the variable footprint torch is pursuing a The diagnostic and computational techniques already Gas-Modulated Plasma Arc approach. Characteristics developed under this project now represent the state of of the new hardware include decoupled heat and filler the art in this area. metal delivery, variable heat output distribution and modular construction for multi-functionality. A During the next five years of this project, we propose to physically-based model is currently under development further extend and generalize these techniques to permit as an aid in designing an appropriate controller for the their application to several additional topics of timely said torch. The model will be tested and verified upon importance in the thermal plasma processing of completion of the torch, currently under in-house materials, namely (1) functionally gradient materials fabrication. (FGMs), (2) reactive plasma spraying, and (3) plasma chemical synthesis of nanophase materials. These

82 Office of Energy Research

In the area of distributed parameter control, we are 166. THERMAL PLASMA CHEMICAL VAPOR considering both the basic modeling form along with a DEPOSITION OF ADVANCED MATERIALS multivariable optimal control philosophy. Techniques $157,975 are being developed for optimally locating and shaping DOE Contact: Robert E. Price, (301) 903-5822 (in space and time) heating/cooling sources (e.g., University of Minnesota Contact: J. Heberlein cooling passages in a mold). The theory for optimal location of measurements has been studied, and The objectives of this program include the charac- simulations and experiments were conducted to study terization of plasma reactors used for materials the findings. As an example application, transient processing in particular for the deposition of diamond temperature control was implemented on a model used films and the generation of ultrafine particles. by Bethlehem Steel Corporation for a hot slab mill. The techniques being developed are being used as For characterizing a particular diamond deposition guidelines for developing new actuators (heaters, reactor, a realistic model has been developed for liquid torches etc.) and sensors for a variety of industrial precursor injection into the plasma in front of the processes. substrate. This three-dimensional model is based on a fluid dynamic description of the plasma jet and the Keywords: Gas-Metal Arc, Welding injection gas streams, an energy transfer model including evaporation of the droplets, dissociation of the 165. METAL TRANSFER IN GAS-METAL ARC vapors, and recombination reactions according to WELDING chemical kinetics. A surface kinetics model describes $124,000 the diamond film growth. Initial results show reasonable DOE Contact: Robert E. Price, (301) 903-5822 agreement with experiments. MIT Contacts: T. W. Eagar and J. Lang, (617) 253-3229 The theoretical description of rf reactors for ultrafine powder production has been completed, and Three projects have been undertaken, all aimed at temperature and velocity profiles for different reactor improved control of the final properties of a weld. configurations and operating conditions provide a basis for future optimal reactor design. The first project, now completed, was a study to model droplet detachment dynamics. Experimental data was In order to meet needs for spatially and temporally generated using a specially developed GMAW system resolved measurements of the characteristics of with laser imaging, high speed video, and electrode turbulent plasma jets, a diagnostic capability has been vibration mechanics. Simulations based on a lumped established based on laser scattering techniques. parameter model were also conducted and good results Results of these measurements will be compared with with the experiments attained. findings obtained at INEL.

The second project is to develop a semi-transferred For determining transport coefficients of gas mixtures at plasma welding system. This system is presently under plasma temperatures, the influence of different construction. It will consist of two independent plasmas. interaction potentials during binary collisions has been A transferred plasma is used for substrate heating, established and recommendations have been made for while a second non-transferred plasma is used to potentials providing the most reliable data. provide a spray coating stream. Each will be independently controlled with a separate power supply. Keywords: Plasma, CVD, Diamond

The third project is to model and predict the physics of 167. RESEARCH ON COMBUSTION-DRIVEN HVOF the weld pool during GMAW. The first phase of the THERMAL SPRAYS experimental component of this project has been $96,893 completed. The theoretical part is currently under way. DOE Contact: Robert E. Price, (301) 903-5822 Present efforts are focused on determining the shape of Pennsylvania State University Contact: the free surface of the molten metal and its influence in G. Settles, (814) 863-1504 the fluid flow, and the influence of Marangoni flows due to compositional differences between the impinging The High-Velocity Oxy-Fuel (HVOF) thermal spray droplet and the substrate. process combines the fields of materials, combustion, and gas dynamics. It relies on combustion to melt and Keywords: Gas-Metal Arc, Welding propel solid particles at high speeds onto a surface to be coated. The goal of this research is to understand

83 Office of Energy Research

and improve the HVOF deposition of corrosion-resistant means by which macrosegregation may be actively coatings, which are important in many energy-related suppressed, as, for example, through the application of industries. This involves both experimentation and a magnetic field or intermittent rotation of the mold. modeling. Keywords: Mixture, Convection HVOF spraygun nozzle design and operating parameters have been found with which to vary the MATERIALS PROPERTIES, BEHAVIOR, kinetic and thermal energies of the spray particles CHARACTERIZATION OR TESTING independently. Through metallographic analysis, the resulting coating properties are now being studied. The 169. CONTINUUM DAMAGE MECHANICS - ability to do this is apparently unique, with results which CRITICAL STATES are expected to be of direct use to HVOF users. For $ 0 example, it should be possible to tailor coatings to DOE Contact: Robert E. Price, (301) 903-5822 produce desirable properties such as low porosity, high Arizona State Contact: D. Krajcinovic, density, and high corrosion resistance. An early result is (602) 965-8656 that stainless steel particles already molten before impact tend to produce less desirable coatings than Objective: Primary objective of the current research solid particles which fuse upon impact due to their program is to examine a variety of critical states in kinetic energy. mechanical response of brittle and quasi-brittle solids containing a large number of crack-like micro-defects. Results of the research are presented annually at the More specifically, the focus of the ongoing research is National Thermal Spray Conference. One Ph.D. has placed on the determination of circumstances (type of been educated and a second graduate student is loading, confinement level, shape and size of the, currently working on this project. specimen, thermal and environmental conditions, 'etc.) leading to the onset of critical states defined as a Keywords: Combustion, Oxy-Fuel threshold connectivity at which a solid ceases to support external loads. 168. EFFECT OF FORCED AND NATURAL CONVECTION ON SOLIDIFICATION OF Technical Approach: Current applied mechanics/ BINARY MIXTURES engineering practice in evaluating the mechanical $0 . failures of brittle and quasi-brittle solids emphasizes use DOE Contact: Robert E. Price, (301) 903-5822 of effective continuum theories coupled with the Purdue University Contact: F. Incropera, deterministic and highly idealized description of the (317) 494-5688 defect geometry (such as doubly periodic arrays of penny-shaped cracks). In contrast, the approach This study deals with the influence of combined selected in this research program accentuates the convection mechanisms on the solidification of binary stochastic geometry of the microstructural disorder and systems. A major accomplishment of research its effect on the onset of macro-fracture and the type of performed to date has been the development and the failure mode. numerical solution of a continuum model, which uses a single set of equations to predict transport phenomena One of the important aspects of this research is to in the liquid, "mushy" (two-phase), and solid regions of explore applicability of the novel methods of statistical the mixture. Calculations have been performed for physics (percolation theory, models of self-organized aqueous salt solutions and/or lead/tin alloys involving criticality, etc.) to micromechanical models. Some of the forced convection, thermo/solutal natural convection, already obtained results provide connection between the and/or thermo/diffusocapillary convection. The mechanical parameters such as stiffness and damage calculations have revealed a wide variety of rich and variable and the percolation theory concepts such as robust flow conditions, including important physical the order parameter, excluded volume, etc. This features of the solidification process which have been provides a set of rational criteria for the selection of the observed experimentally but have heretofore eluded universal dimensional invariants needed to describe the prediction. These features include double-diffusive onset of a certain class of failures. Secondly, use of the layering in the melt, development of an irregular liquidus statistical methods (such as fractal and multifractal front, remelting of solid, development of flow channels formalism) provide a superior and size-independent in the mushy region, and the establishment of (intrinsic) description of the fluctuations in the stress characteristic macrosegregation patterns (regions of field (stress concentrations) in the vicinity of the critical significantly different composition) in the final solid, states. This aspect alone should provide a definitive Theoretical and experimental studies have also revealed answer related to the dependence of the order-disorder

84 Office of Energy Research transition on the microstructuraltexture and/or boundary two-dimensional geometries. The results illustrate the conditions. In summary, the selected approach provides importance of accounting for nonlinear changes in the best hope of description of the universal aspects of geometry, grain-boundary diffusion processes, elastic the stochastic nature of the damage and its evolution in accommodation of the surrounding material as well as the vicinity of the critical state. more realistic constitutive laws for creep deformation. Current efforts involve investigating different load Keywords: Continuum Mechanics, Fractals, Brittle histories and three-dimensional effects. In addition, the Materials ultimate goal of this effort is to establish a firm connection between the micro- and macro-mechanical 170. AN INVESTIGATION OF HISTORY-DEPENDENT models thereby leading to the development of DAMAGE IN TIME-DEPENDENT FRACTURE appropriate methodology for life prediction of structural MECHANICS components exposed to high temperature conditions $99,729 involving complex load histories. DOE Contact: Robert E. Price, (301) 903-5822 Battelle Memorial Institute Contact: F. Brust, Keywords: Damage, Fracture Mechanics (614) 424-5034 171. INTELLIGENT CONTROL OF THERMAL In order to meet the demand imposed by future PROCESSES technology, new plants with increased energy efficiency $517,000 must operate at relatively high temperatures. DOE Contact: Robert E. Price, (301) 903-5822 Additionally, the existing power generation equipment in Idaho National Engineering Laboratory the United States continues to age and is being used far Contact: J. R. Fincke, (208) 526-2031 beyond its intended life. Some recent failures have clearly demonstrated that the current methods for This project addresses intelligent control of thermal insuring safety and reliability of high temperature processes as applied to gas metal arc welding. equipment is inadequate. Owing to these concerns, a Intelligent control is defined as the combined application thorough understanding of high temperature failure of process modeling, sensing, artificial intelligence, and initiation and propagation in materials exposed to control theory to process control. The intent of intelligent variable mechanical and thermal loading is very control is to produce a good product without relying on important. post-process inspection and statistical quality control procedures, by integrating knowledge of process In the past, the evolution of damage has been engineering practice and process physics into sensing addressed through a macroscopic theoretical model and control algorithms. The gas metal arc welding (developed as part of this effort) which attempt to process is used as a model system; considerable predict the crack growth and failure response of fundamental information on the process has been material components exposed to high temperature developed at INEL and MIT during the past ten years. conditions. However, micromechanical processes such Research is being conducted on analytical modeling of as diffusion of atomic flux into grain boundaries, elastic nonlinear aspects of molten metal droplet formation and accommodation and creep deformation of the material transfer, and integration of knowledge-based control and grain boundary sliding do contribute significantly to methods (including artificial neural networks and fuzzy the nucleation and growth of voids leading to failure. logic based connectionist systems) with iterative Understanding gained by consideration of micro- learning control methods. Results are being transferred mechanics of cavity growth is crucial for developing to industrial partners through a related EE-OTT CRADA damage-based constitutive models as well as on Intelligent Diagnostics, Sensing, and Control of Thin methodologies for life prediction of structural Section Welding. components. While the application of this understanding in estimating life of structural materials experiencing New work has been started on control methods for high temperature creep has met with some success, it distributed thermal processes. The focus of this work is is of limited use for structural components experiencing specifically on processes employing one or more point complex load histories under high temperature sources of heat and or mass with spatial rastering and conditions. temporal modulation of the source(s) to produce a distributed temperature field in a distributed mass. The A micro-mechanical model accounting for rate- prototypical process is plasma hearth melting of metals. controlling microscopic processes has been developed The initial work is investigating iterative learning control as part of this effort. To date, both sustained and to control the trajectory of a heat source through state variable load histories have been investigated in

85 Office of Energy Research space (including both the spatial terajectory of the heat presently in progress. Testing of fracture toughness source and the thermal parameter trajectory). specimens, specimens containing surface cracks, and modified specimen geometries is planned for the future. This project is part of a collaborative research program with the Massachusetts Institute of Technology. Keywords: Fracture Mechanics, Welding

Keywords: Fuzzy Logic, Neural Networks 173. NONDESTRUCTIVE EVALUATION OF SUPERCONDUCTORS 172. ELASTIC-PLASTIC FRACTURE ANALYSIS $205,000 EMPHASIS ON SURFACE FLAWS DOE Contact: Robert E. Price, (301) 903-5822 $132,000 Idaho National Engineering Laboratory DOE Contact: Robert E. Price, (301) 903-5822 Contact: K. L. Telschow, (208) 526-1254 Idaho National Engineering Laboratory Contacts: W. G. Reuter, J. Epstein, This project is concerned with the development and W. Lloyd, (205) 526-0111 application of new nondestructive evaluation (NDE) techniques and devices for the characterization of The objective is to improve design and analytical materials, particularly high-temperature supercon- techniques for predicting the integrity of flawed ducting materials in tape form. Microstructural and, structural components. The research is primarily particularly, superconducting properties, need to be experimental, with analytical evaluations guiding the measured noninvasively and spatially in order to aid the direction of experimental testing. Tests are being fabrication process. conducted on materials ranging from linear elastic to fully plastic. The latter extends beyond the range of a Two approaches that are both noncontacting and J-controlled field. Specimens containing surface cracks potentially applicable to the industrial environment are are used to simulate the fracture process (crack growth being investigated separately and together. One initiation, subcritical growth, and catastrophic failure) approach uses noncontacting induced current for that may occur in structural components. determination of critical currents on a local scale. This technique can be used alone or in conjunction with Metallography and microtopography techniques have external applied fields and DC transport currents to been developed to measure crack tip opening determine spatial variations in critical current density. displacement and crack tip opening angle for Its operation is based on inducing the critical state and comparison with analytical models. Moire interferometry determining full penetration through the tape with a techniques are used to evaluate and quantify the small probe coil. A new integral equation approach has deformation in the crack region. These studies have been found and solved iteratively that determines the resulted in the ability to predict crack growth initiation of flux front profile in geometries with azimuthal symmetry specimens containing surface cracks using constraint accounting for demagnetization effects. The capability and fracture toughness data obtained from standard of high temperature SQUID sensors for measurements fracture toughness specimens. Results are being in long length tapes is being investigated for increased transferred to industry in the form of an ASTM Test sensitivity and full hysteresis behavior determination. Standard on Surface Cracked Specimens (Structures) The second approach uses lasers to generate and that is presently being developed. Future research will detect ultrasonic wave modes in tape geometries. focus on predicting the stable crack growth process in Specific elastic wave modes are employed both base metal and in weldments. analytically and experimentally to determine layer thickness, elastic constants and grain orientation. The Due to the complexity of studying the fracture process in stability of the critical state to elastic strain is being weldments, diffusion bonded specimens were used investigated using both approaches simultaneously in a initially to simulate a weldment. This provided an coupled mode. opportunity to study the fracture process in a model weldment (two dissimilar materials, e.g., base metal Keywords: Nondestructive Evaluation, Super- and weld metal) of either a butt weld or a single "V' conductors groove geometry that contained neither a heat affected zone nor residual stresses. This work has been completed and now the focus is on actual weldments of A710 steel. Two weldments have been fabricated with one having matched weld metal and the second an overmatched weld metal. Characterization of the microstructure and of local tensile properties is

86 Office of Energy Research

174. ORIGINS OF ASYMMETRIC STRESS-STRAIN material resistance to both ductile hole growth and RESPONSE IN PHASE TRANSFORMATIONS cleavage fracture mechanisms provide additional $80,535 complexity, compared to the corresponding fracture DOE Contact: Robert E. Price, (301) 903-5822 mechanics models of macroscopically homogeneous University of Illnois Contact: H. Sehitoglu, crack-tip microstructures and properties. (217) 333-4112 Under macroscopic mode I loading, strength- A number of uniaxial and stress state experiments on mismatched interface crack-tip stress and deformation the NiTi alloys that are known to undergo thermo-elastic fields show considerable differences from the phase transformations were conducted. Unlike steels corresponding fields in mechanically homogeneous which exhibit virtually no recoverable transformation media. In particular, both triaxial stress and plastic strains, the transformation strains in this class of strain levels in the softer domain (e.g., an under- materials are partially recovered upon unloading, matched baseplate) are elevated. Families of depending on the applied strain levels. Using a mismatched fields have been characterized by finite servohydraulic intensifier, a servohydraulic test element and slip-line solutions, and have been shown to machine, and a novel pressurized test chamber; apply from small-scale yielding through fully-plastic pressures of 750MPa and axial stresses of almost any conditions. magnitude are simultaneously generated and applied to the gage section of a solid, cylindrical NiTi specimens. The mismatched fields are being coupled with local The work utilizes a robust internal load cell that can models of cleavage and ductile fracture in the measure axial forces without the effect of seal friction inhomogeneous crack-tip region, and the results and demonstrate innovative ways of calibrating this load compared with experiments on both model weldments cell, and methods of axial and circumferential strain created by diffusion-bonding and with actual welds in measurement in a pressure environment and verify A710 steel. accuracy of these results. Constitutive models proposed in the literature for thermo-elastic transformation were Keywords: Fracture Mechanics, Welding evaluated in light of these results. The current models predict that the volume fraction of martensite is solely 176. DEVELOPMENT OF MEASUREMENT CAPA- dependent on the effective stress. Our experimental BILITIES FOR THE THERMOPHYSICAL results indicate that there is a dependence of the PROPERTIES OF ENERGY-RELATED FLUIDS transformations strain on the hydrostatic stress $425,000 component with strong asymmetry in tension versus DOE Contact: Robert E. Price, (301) 903-5822 compression. In view of these experimental findings, National Institute of Standard and Technology new transformation models are being developed Contacts: R. Kayser and W. Haynes, incorporating the low symmetry of the twinning planes. (301) 975-2583 The stress-induced phase transformation of CuZnAI was also found to be stress state dependent but less so The major objectives of this new three-year project are than NiTi. to develop state-of-the-art experimental apparatus for measuring the thermophysical properties of a wide Keywords: Alloys, Phase Transformations range of fluids and fluid mixtures important to the energy, chemical, and energy-related industries. The 175. MODELING AND ANALYSIS OF SURFACE specific measurement capabilities to be developed are CRACKS the following: Small-Volume, Dual-Cell Dew-Bubble $192,000 Point Apparatus; Heat-of-Vaporization Calorimeter and DOE Contact: Robert E. Price, (301) 903-5822 Effusion Cell for Vapor-Pressure Determinations; MIT Contacts: David M. Parks, (617) 253-0033 Solubility Measurements Using Magnetic Levitation; and F. A. McClintock, (617) 253-2219 Thermal Diffusivity from Light Scattering; and Phase- Equilibria Apparatus for Azeotropic Aqueous-Organic- We are developing a mechanics basis for analyzing the Salt Mixtures. These new apparatus will extend fracture behavior of cracks located on or near the fusion significantly the state of the art for properties zones of structural weldments. Such welds are often measurements and make it possible to study a wide characterized by significant strength mismatch between range of complex fluid systems (e.g., highly involatile, base plate and weld metal, as well as by local strength very insoluble, highly polar, electrically conducting, gradients associated with metallurgical details of the heat-affected zones. Moreover, the local gradients in microstructure, and the accompanying gradients in

87 Office of Energy Research reacting) under conditions which have been previously 178. THIN FILM CHARACTERIZATION AND FLAW inaccessible. DETECTION $0 Keywords: Thermophysical Properties, Fluids DOE Contact: Robert E. Price, (301) 903-5822 Northwestern University Contact: 177. HIGH-T. SUPERCONDUCTOR- J. D. Achenbach, (312) 491-5527 SEMICONDUCTOR INTEGRATION AND CONTACT TECHNOLOGY This work is concerned with the determination of the $116,800 elastic constants of thin films deposited on substrates, DOE Contact: Robert E. Price, (301) 903-5822 with the measurement of residual stresses in such films National Institute of Standard and Technology and with the detection and characterization of defects in Contacts: J. Moreland, (303) 497-3641 and thin film substrate configurations. J. W. Elkin, (303) 497-5448 There are many present and potential applications of The purpose of this project is to study materials configurations consisting of a thin film deposited on a problems faced in integrating high-T, superconductor substrate. Thin films that are deposited to improve the (HTS) thin-film technology with conventional semi- hardness and/or the thermal properties of surfaces are conducting technologies. The emphasis of the research of principal interest in this work. Thin film technology is to investigate HTS-semiconductor contact systems does, however, also include high Tc superconductor and novel HTS-semiconductor devices. The ultimate films, films for magnetic recording, superlattices and goal is to develop HTS thin-film technology to its fullest films for band-gap engineering and quantum devices. potential for multi chip module interconnections, future The studies carried out on this project also have ULSI source and drain connections, and microelectronic relevance to those applications. microwave filters. These potential applications provide the motivation for a thorough investigation of HTS thin- Both the film and the substrate are generally film materials development of these hybrid systems. anisotropic. A line-focus acoustic microscope, is being Determining the compatibility of HTS thin-film used to measure the speed of wave modes in the thin deposition and patterning processing with that of film/substrate system. This microscope has unique standard Si processing is crucial for expanding the advantages for measurements in anisotropic media. applications of these hybrid technologies. Analytical and numerical techniques are employed to extract the desired information on the thin film from the The nanostuctural properties of HTS materials have measured data. Recent results include: (1) use of proven to have a principal influence on the electrical multiple wave modes to determine thin film constants, properties of HTS materials and devices. For this (2) measurements of superlattice film constants, and (3) reason the use of scanned probe microscopies are investigation of the effect of surface roughness. being emphasized for evaluating HTS-semiconductor epitaxy as well as electrical conduction in interconnects Keywords: Thin Films, Superlattices, Surface and contacts to hybrid device structures. The further Roughness development of scanned probe microscopies, specifically for electronic device imaging will be 179. TRANSPORT PROPERTIES OF DISORDERED invaluable not only for the HTS-semiconductor POROUS MEDIA FROM THE integration studies but for all developments in MICROSTRUCTURE microelectronics in the foreseeable future. The current $116,959 emphasis is on developing scanning potentiometry DOE Contact: Robert E. Price, (301) 903-5822 based on atomic force microscopy with resolution and Princeton University Contact: S. Torquato, sensitivity levels better than 50 nm and 1 mV, (609) 258-4600 respectively. Also, investigations regarding adapting scanning potentiometry for high frequency applications This research program is concerned with the up to 100 GHz are under way. quantitative relationship between transport properties of a disordered heterogeneous medium that arise in Keywords: High Tc Superconductors, Contacts various energy-related problems (e.g., thermal or electrical conductivity, trapping rate, and the fluid permeability) and its microstructure. In particular, we shall focus our attention on studying the effect of porosity, spatial distribution of the phase elements, interfacial surface statistics, anisotropy, and size distribution of the phase elements, on the effective

88 Office of Energy Research properties of models of both unconsolidated media deformed into metal with elastic and inelastic (e.g., soils and packed beds of discrete particles) and orthotropy. Simulation of this process is underway. consolidated media (e.g., sandstones and sintered materials). The small strain version of VBO has been extended to high homologous temperature and applied to Alloy 600 Both theoretical, computer-simulation, and H at temperatures above 0.7. The model can simulate experimental techniques have been employed to the experimentally observed creep and tensile behavior. quantitatively characterize the microstructure and It is also shown that the transition from the solid to the compute the transport properties of disordered media. fluid state can be accomplished easily with VBO. Statistical-mechanical theory has been used to obtain Applications to solder materials for which ambient n-point distribution functions and to study percolation temperature is a high homologous temperature and an phenomena in continuum random-media models. For effort to reduce the number of needed constants in the example, the pore-size distribution, lineal path function, model are underway. and the chord-length distribution function have been investigated and computed. This has led to accurate Keywords: Deformation, Viscoplasticity predictions of transport properties of realistic models of isotropic as well as anisotropic heterogeneous media. 181. STRESS AND STABILITY ANALYSIS OF Cross property relations have been derived. Rigorous SURFACE MORPHOLOGY OF ELASTIC AND relations which link the fluid permeability to length PIEZOELECTRIC MATERIALS scales obtainable from Nuclear Magnetic Resonance $137,000 experiments and the effective electrical conductivity DOE Contact: Robert E. Price, (301) 903-5822 have been derived. Moreover, the effective conductivity Stanford University Contacts: H. Gao and has been related to the effective elastic moduli. D. Barnett, (415) 725-2560 Recently, 3-D images of a sandstone have been obtained using X-ray tomographic techniques and The objective of this research has been to study statistical corrleation funcations have been extracted morphological stabilities and instabilities in elastic and from them. piezoelectric solid. In morphologies are included surface shapes, cracks, and defect patterns. In this past year Keywords: Porous Media, Transport Properties the conditions for stability or instability of surfaces and interfaces in piezoelectric materials (including arbitrary 180. INELASTIC CONSTITUTIVE EQUATION: elastic and piezoelectric anisotropy) have been DEFORMATION INDUCED ANISTROPY AND developed.' This work has shown that piezoelectric THE BEHAVIOR AT HIGH HOMOLOGOUS coupling may tend to either stabilize or destabilize an TEMPERATURE initial flat boundary or interface. A destabilized surface $149,828 evolves toward the formation of crack-like flaw. This DOE Contact: Robert E. Price, (301) 903-5822 study suggests that piezoelectric coupling could be Rensselaer Polytechnic Institute Contact: utilized to control diffusive initiation of surface defects. A Erhard Krempl, (518) 266-6432 portion of future work will be directed toward corroborating theory with experiments and identifying Using experimental results obtained with computer- whether more sophisticated theoretical models for controlled, servohydraulic testing machines, continuum defect generation need to be explored. Another direction mechanics and materials science as backgrounds, which this research has taken is the study of fracture in constitutive equations (mathematical models of material piezoelectric solids. A strip saturation model and the deformation behavior that are used in stress and concept of multiscale energy release rates have been life-time analyses) are being developed with emphasis on two aspects: Deformation induced anisotropy for large deformation on the one hand and high homologous temperature on the other. Both areas extend the modeling capability of the previously developed "unified," state variable viscoplasticity theory based on overstress (VBO).

A mathematical framework and a formulation for the representation of deformation induced anisotropy has 'N. Y. Chien, H. Gao, G. Herrmann, and D. M. been developed and this theory is now being applied to Barnett, "Diffusive Surface Instabilities Induced by rolling of metals. In this case an isotropic metal can be Electromechanical Loading," Proceedings of the Royal Society, London, A452, pp. 527-541 (1995).

89 Office of Energy Research

introduced 1 to explain some existing experimental YBCO near the transition point yield curves as a observations of the behavior of cracks in piezoelectric function of temperature with shapes that are very ceramics. Extensions of this work are underway. different, depending on the polarization of the probe beam relative to the A and B directions. Twinned Patterns of equilibrium 2-dimensional arrangements of samples do not show this anisotropy. The shape and large numbers of dislocations have been computed by sign of these curves also appears to provide a very using numerical methods to minimize the potential sensitive measurement of the state of doping of the energy of the dislocation distributions. Efficiency of material. By measuring the modulated signals at the computation has been greatly enhanced by studying second harmonic of the input signal, the temperature doubly periodic arrangements of dislocation cells for modulation of the sample by the laser beam can be which some analytic reduction is possible. It has been determined. During the last year the system has been found that many possible equilibrium patterns exist rebuilt to give more accurate results, to work at lower under zero applied stress, i.e., nearby equilibrium temperatures so that we can make measurements of arrangements are always available. A study of the normal superconductors and compare with theory, and stabilty of these arrays under application of applied to make more rapid measurements of the quality of thin stresses is now underway. film superconductors.

Keywords: Surfaces, Interfaces, Stress Analysis, Keywords: High Tc Superconductors, Thin Films Piezoelectrics 183. 3-D EXPERIMENTAL FRACTURE ANALYSIS AT 182. OPTICAL TECHNIQUES FOR CHARACTERI- HIGH TEMPERATURES ZATION OF HIGH TEMPERATURE $76,721 SUPERCONDUCTORS DOE Contact: Robert E. Price, (301) 903-5822 $231,000 University of Washington Contact: DOE Contact: Robert E. Price, (301) 903-5822 Albert Kobayashi, (206) 543-5488 Stanford University: G. S. Kino, (415) 497-0205 The objective of this three year project is to assess experimentally, the validity of T* integral and its Photothermal techniques are used to measure the applicability to quasi-static and dynamic ductile fracture. normal carrier density below the transition temperature Early in the second year, a protocol for extracting the T* Tc in high-temperature superconductors, to study the integral values fromthe surface displacement fields nature of the phase transition, and to measure the obtained by moire interferometry was established. The homogeneity and quality of these materials. A procedure consists of numerically evaluating the modulated focused laser beam incident on the sample integral along a partial contour, a small distance, e, in varies its temperature periodically, and a second probe front of the crack tip, In order to assure a state of plane beam a few microns away measures the differential stress, e is equated to one plate thickness and the reflectivity associated with the thermal wave resultant T* is designated T*e. The procedure was propagating along the sample. Changes in critical verified through numerical experiments conducted at the temperature in regions less than 100 pm apart have Georgia Institute of Technology (GIT) under a parallel been measured, and the difference in quality of different DOE grant. samples can clearly be seen. Measurement of thermal diffusivity in single-YBCO crystals yields good estimates The established procedure was used to determine T*e's of the variation of normal electron density with of A606 HSLA steel, single-edge notched (SEN) temperature. Observations of small changes in the specimens with small stable crack growth, = 2 mm, and phase variation yield the transition temperature of the 2024-T3 aluminum, compact (CT) of large crack material. Polarized light observations of single-crystal growth, = 8 mm. Parallel numerical analysis of these two sets of experiments were conducted at GIT where the experimentally and numerically determined T*e were found to be in excellent agreement. T* c of the A606 'H. Gao, T.-Y. Zhang, and P. Tong, "Local and HSLA SEN specimen continued to increase with stable Global Energy Release Rates for an Electrically Yielded crack growth, possibly due to the lack of constraint in Crack in Piezoelectric Ceramics," Journal of the the SEN specimen. T*c of the 2024-T3 CT specimen Mechanics and Physics of Solids (in review). reached a steady state value of · 140 MPa-mm. The CT specimen results suggest that T*C could be a viable 2H. Gao and D. M. Barnett, "An Invariance Property fracture parameter which controls stable crack growth. of Local Energy Release Rates in a Strip Saturation The crack tip opening angles (CTOA) for the two Model of Piezoelectric Fracture," International Journal of materials immediately reached steady state values with Fracture (in review).

90 Office of Energy Research crack growth. However, results from a FAA funded DEVICE OR COMPONENT FABRICATION, study showed that CTOA is insensitive to the inherent BEHAVIOR OR TESTING decrease in ductility due to increased thickness and therefore may not be a proper fracture parameter. 185. AN ANALYTICAL-NUMERICAL ALTERNATING METHOD FOR 3-D INELASTIC FRACTURE AND Keywords: Fracture Mechanics, Crack Growth INTEGRITY ANALYSIS OF PRESSURE- -VESSELS AND PIPING AT ELEVATED 184. SIMULATION AND ANALYSIS OF DYNAMIC TEMPERATURES FAILURE OF DUCTILE MATERIALS $85,000 $99,410 DOE Contact: Robert E. Price, (301) 903-5822 DOE Contact: Robert E. Price, (301) 903-5822 Georgia Institute of Technology Contact: Brown University Contact: B. Freund, S. Atluri, (404) 894-2758 (401) 863-1157 Current and future power generation plants require A central goal in the mechanics of materials is the efficient operation so that energy savings may be determination of parameters which characterize realized. In addition, power generation equipment in the macroscopic failure of materials in terms quantifiable US continues to age, creating operational dangers for characteristics of their microstructure. The motivation is the working staff as well as greater potential for power to establish which characteristics account for outages. Current methods to ensure safe operation of macroscopic failure, with a view toward improvement of these plant components which operate in the nonlinear failure resistance through material selection or material regime are simplistic, and hence, not very microstructural design. In the present project, emphasis reliable. This program is developing advanced analytical is on the behavior of ductile structural alloys under high tools which can be used to reliably assure safety of rate loading conditions. Thus, the dominant mechanism future plants as well as aging plants. The finite element of plastic deformation is crystallographic slip and alternating method is the state-of-the-art methodology material strength degrades through nucleation, growth for determining stress intensity factors for two and three and coalescence of micro-voids. Plastic strains in such dimensional crack growth problems. This method has processes can be large and strain localization is permitted accurate and simple analyses of linear common. The approach is to adapt methodologies for fracture problems to be made so that sophisticated analysis of elastic-viscoplastic systems to problems reliability assessments of operating equipment may be selected on the basis of their relevance to safety of made. This program has extended the finite element pressure vessel and piping systems, to materials alternating method so that it may now be used in the processing and metal forming technologies, and to nonlinear regime, i.e., the non-linear finite element structural reliability under dynamic loading. Initial alternating method. With this new methodology, emphasis has been on failure of an explosively loaded sophisticated damage and fracture assessments can be ring expanding under plane strain conditions, a made for components which experience failures in the configuration which has been studied experimentally. elastic-plastic and high temperature creep regime. This Calculations reveal that strain localization sites, or is truly a revolutionary advance to the fracture necks, are more pervasive under rapid loading, and the assessment field. spacing of necks decreases with increase in loading rate. The influence of inertia on bifurcation of Currently, sophisticated fracture assessments are being deformation states is also being investigated made using advanced fracture theories such as the T*- theoretically. The project is being carried out in integral which were previously unattainable. The collaboration with colleagues involved in experimental methods are being verified by comparison of predictions research on dynamic ductile failure at the California to experimental results. It is anticipated that these Institute of Technology. advances will permit the designer to make sophisticated fracture assessments in the future with a minimum of Keywords: Dynamic Failure, Ductile Materials effort.

Keywords: Fracture, Pressure Vessels, Piping

91 Office of Energy Research

186. PULSE PROPAGATION IN INHOMOGENEOUS magnetic field, and to understand the nature of the OPTICAL WAVEGUIDES phase transitions between them. $200,493 DOE Contact: Robert E. Price, (301) 903-5822 Particular attention has recently been given to studying University of Maryland Contact: C. Menyuk, the equilibrium fluctuation of vortex lines in models of (301) 455-3501 bulk high temperature superconductors.

We are presently working on two principal projects. Simulations have shown that there can be two distinct First, we are studying randomly varying birefringence in phase transitions describing the superconducting optical fibers and its impact on both soliton and NRZ ordering parallel versus perpendicular to the applied communications. We have derived a set of equations magnetic field. The loss of order in the perpendicular (modified Manakov equations) that allow us to simulate direction has been associated with a melting of the the propagation through a fiber with rapidly and ground state vortex line lattice. The loss of order in the randomly varying birefringence on the much longer parallel direction has been associated with the onset of length scale on which the signals varying due to chro- a vortex line tangle percolating throughout the entire matic dispersion, polarization mode dispersion, and system. New simulations, relaxing earlier approxima- nonlinearity. These equations also yield considerable tions, are being carried out to clarify this issue. The physical insight into the behavior of these systems. We effect of applied currents and random vortex pinning have benchmarked these codes carefully, and we have sites will be added in future work. The dynamic behavior demonstrated that they yield the same results as of vortices in two dimensional Josephson arrays has computer codes that use far shorter step sizes and are also recently been investigated using a detailed finite far less efficient. In addition to Monte Carlo methods, size analysis to verify proposed scaling equations. we are now using analytical methods based on the theory of stochastic differential equations to completely This research will greatly enhance the fundamental characterize the probability distribution functions for the understanding of behavior in strongly fluctuating evolution of the signal's state of polarization and the superconducting materials. The results will have impact corresponding terms in the modified Manakov equation in understanding the magnetic properties of the new that describes the complete evolution, high temperature superconductors, and in the design of Josephson junction arrays for use as microwave The second project is quasi-phase-matched detectors and generators. waveguides. We are using a Green's function approach to determine the rate at which radiation leaks from the Keywords: Superconductors, Flux Flow, Josephson quasi-phase-matched guides. In the future we will look Junctions at oblique guides and guides with other unusual cross-sections that appear in the experiments to reduce GEOSCIENCES RESEARCH unwanted Bragg reflections. The BES Geosciences Research Program supports Keywords: Optical Waveguides, Monte Carlo research that is fundamental in nature and of long-term relevance to one or more energy technologies, national 187. FLUX FLOW, PINNING AND RESISTIVE security, energy conservation, or the safety objectives of BEHAVIOR IN SUPERCONDUCTING the Department of Energy. It is also concerned with the NETWORKS extraction and utilization of such resources in an $71,930 environmentally acceptable way. The purpose of this DOE Contact: Robert E. Price, (301) 903-5822 program is to develop geoscience or geosciences- University of Rochester Contact: S. Teitel, related information in support of one or more of these (716) 275-4039 Department of Energy objectives or to develop the broad, basic understanding of geologic materials and The fluctuation of vortices and vortex lines has been processes necessary for the attainment of long-term shown to be a major source of electrical resistance for Department of Energy goals. In general, individual superconducting networks when placed in magnetic research efforts supported by this program involve fields. Systems of particular interest include the new elements relevant to several different energy objectives. high temperature type II superconductors, and periodic The DOE contact for this Program is Paula M. arrays of Josephson junctions. Numerical simulations Davidson, (301)903-5822. are being carried out to identify and characterize the nature of the various vortex structures present in such systems, as a function of temperature and applied

92 Office of Energy Research

MATERIALS PREPARATION, SYNTHESIS, fluid exchange obtained from natural samples, in order DEPOSITION, GROWTH OR FORMING to help determine a mechanistic understanding of the exchange rates over both short and longer time periods 188. AN INVESTIGATION OF ORGANIC accessible in the sedimentary record. ANION-MINERAL SURFACE INTERACTIONS DURING DIAGENESIS $200,000 Keywords: Carbonate Minerals, Dissolution and DOE Contact: PM. Davidson, (301) 903-5822 Precipitation Mechanisms SNL Contact: Patrick Brady, (505) 844-7216 and Randall Cygan 190. TRANSITION METAL CATALYSIS IN THE GENERATION OF PETROLEUM AND The research is to investigate adsorption of anionic NATURAL GAS carboxylate and phenolate groups onto aluminosilicate $109,313 surfaces in order to evaluate the role of organic acids as DOE Contact: P. M. Davidson, (301) 903-5822 (1) catalysts for mineral dissolution and porosity Rice University Contact: Frank D. Mango, evolution in deep basins, and (2) controlling agents of (713) 527-4880 coupled dissolution and growth of during diagenesis. Combined experimental and theoretical approaches are Light hydrocarbons in petroleum, including natural gas used to investigate the mechanisms and reaction rates (C,-C4 ), are conventionally viewed as products of of organic anion adsorption. T-dependent adsorption of progressive thermal breakdown of kerogen and oil. oxalate, acetate, salicylate and benzoate anions onto Alternatively, transition metals, activated under the selected aluminosilicate surfaces are being measured, reducing conditions of diagenesis, can be proposed as as are dissolution rates of alumina (as corundum), catalysts in the generation of light hydrocarbons. tremolite, albite, kaolinite and precipitation rates of Transition metal-rich kerogeneous sedimentary rocks kaolinite, in solutions containing various organic acids, were reacted under reducing conditions at temperatures at temperatures of 30-90°C. Theoretical investigations for which the substrates alone, N-octadecene + are testing mechanistic connections between hydrogen, are stable indefinitely. Catalytic activity was 7 metal-anion complexation, anion adsorption, and measured to be on the order of 10- g CH4/d/g kerogen, mineral growth with the new experimental data. The suggesting robust catalytic activity over geologic time at influence of surface-site chemistry and bonding are moderate sedimentary temperatures. being investigated, in an attempt to establish general crystal-chemical rules for predicting the extent of Keywords: Transition Metals, Catalysis, Petroleum organically-controlled reactions during diagenesis. 191. MINERAL DISSOLUTION AND PRECIPITATION Keywords: Surface reactions, Aluminosilicate KINETICS: A COMBINED ATOMIC-SCALE AND Minerals, Adsorption Mechanisms MACRO-SCALE INVESTIGATION $181,477 189. SOLUTION-REPRECIPITATION OF CALCITE DOE Contact: P M. Davidson, (301) 903-5822 AND PARTITIONING OF DIVALENT METALS University of Wyoming Contact: $129,999 Carrick M. Eggleston, (307) 766-6769 DOE Contact: P. M. Davidson, (301) 903-5822 Lawrence Livermore National Laboratory University of Chicago Contact: Frank M. Richter, Contact: Kevin G. Knauss, (510) 422-1372 (773) 702-8118 The project combines atomic-scale and macroscale The proposed research is to investigate the exchange of approaches for investigating mineral-fluid interactions, metals (principally Sr and Cd) between CaCO 3 and in order to provide improved understanding of mineral fluids, at a fundamental level necessary for basing dissolution and precipitation processes. With the thermodynamic and kinetic treatments of dissolution/ development of a high temperature flow-through atomic reprecipitation. The proposed measurements of force microscope (AFM), atomic-scale kinetic precipitation rates and exchange of Sr and Cd with experiments will be possible under geologically relevant calcite solid-solutions will serve as the basis for conditions for important oxide and aluminosilicate developing a more general treatment of governing minerals. Macroscopic measurements of dissolution/ mechanisms and kinetics of dispersion of tracers and precipitation rates, activation energies, and rates of step contaminants uptake/release in calcites, the motion across surfaces, performed under identical predominant constituents of limestones. Laboratory conditions, will provide the basis for addressing open measurements of exchange rates are to be questions concerning the macroscopic rate laws and complemented with analyses of the record of calcite- microscopic and interpretations, in terms of dissolution

93 Office of Energy Research

and precipitation mechanisms, and nature of the topes between CO2 vapor and rhyolitic glass and melt reactive interface. was measured. The kinetics of OH-forming reactions in silicate glasses were studied. Diffusion of water in Keywords: Atomic Force Microscopy, Silicate basaltic melts and of water and CO2 in rhyolitic glasses Minerals, Dissolution and Precipitation and melts was studied. Results were used to un- Mechanisms derstand oxygen 'self-diffusion' in silicate minerals and glasses and enhanced oxygen diffusion under hy-. MATERIALS STRUCTURE AND COMPOSITION drothermal conditions.

192. REACTION MECHANISMS OF CLAY Keywords: Infrared Spectroscopy, Silicate Minerals, MINERALS AND ORGANIC DIAGENESIS: AN Glasses, Silicate Liquids, Speciation HRTEMIAEM STUDY $139,065 194. BIOMINERALIZATION: SYSTEMATICS OF DOE Contact: P. M. Davidson, (301) 903-5822 ORGANIC-DIRECTED CONTROLS ON Arizona State University Contact: P. R. Buseck, CARBONATE GROWTH MORPHOLOGIES AND (602) 965-3945 KINETICS DETERMINED BY In situ ATOMIC FORCE MICROSCOPY The research is to investigate the structures of $38,559 fine-scale diagenetic material using high-resolution DOE Contact: P. M. Davidson, (301) 903-5822 transmission electron microscopy/analytical electron Georgia Inst. Of Technology Contact: P. Dove, microprobe (HRTEM/AEM) techniques which will (404) 894-6043 facilitate in situ identification and evaluation of reaction mechanisms. As a basis for kinetic models this The research is to investigate biomineralization information is used to predict basinal diagenetic mechanisms of dissolution and precipitation reactions patterns for resource exploration. Structural analyses of of the two common calcium carbonate polymorphs, intergrown product and reactant from three principal calcite and (metastable) aragonite. Experiments have diagenetic reactions operative in the formation of been undertaken to monitor surface reaction hydrocarbon reservoirs are proposed: (1) berthierine to morphology and kinetics in the presence of isolated chamosite, (2) smectite to illite, and (3) maturation of simple acidic and basic amino acids, that are kerogen to form oil and gas. candidates for directing growth in natural systems. In order to characterize dynamic nanoscale growth Keywords: Diagenetic Reactions, High-Resolution morphologies and mechanisms, atomic force Transmission Electron Microscopy, microscopy (AFM) observations have been made under Kerogen, Smectite, Illite, Berthierine, in aquo conditions. The combination of.proposed Chamosite mechanism and rate determinations are important for understanding and predicting controls by organic 193. INFRARED SPECTROSCOPY AND HYDROGEN molecules on natural precipitation and dissolution of ISOTOPE GEOCHEMISTRY OF HYDROUS calcite and aragonite, and provide new constraints on SILICATE GLASSES models of bonding and reactivity at the nanoscale in $141,634 organized structures. DOE Contact: P. M. Davidson, (301) 903-5822 Caltech Contacts: S. Epstein, (818) 356-6100 Keywords: Biomineralization, Calcium Carbonate, and E. Stolper, (818) 356-6504 Atomic Force Microscopy, Surface Reactions The focus of this project is the combined application of infrared (IR) spectroscopy and stable isotope 195. REACTIONS AND TRANSPORT OF TOXIC geochemistry to the study of dissolved components in METALS IN ROCK-FORMING SILICATES AT silicate melts and glasses. Different species of dissolved 25°C water and carbon dioxide (e.g., molecules of H20 and $200,000 hydroxyl groups, molecules of CO2 and carbonate ion DOE Contact: P. M. Davidson, (301) 903-5822 complexes) have been analysed to understand volatile Johns Hopkins University Contact: D. R. Veblen, transfer reactions in liquids and glasses. The partition- (410) 516-8487 ing of H isotopes between vapor and hydroxyl groups Lehigh University Contact: E. Ilton, and molecules of H20 dissolved in rhyolitic melts was (610) 758-5834 measured. Concentrations of H20 and CO2 in volcanic glasses and CO2 in rhyolitic liquid were measured at Heterogeneous electron-cation transfer reactions pressures up to 1500 bars. The fractionation of O iso- between aqueous metals and silicates can be

94 Office of Energy Research responsible for the retention or mobilization of MATERIALS PROPERTIES, BEHAVIOR, multivalent cations in the near-surface environment. CHARACTERIZATION OR TESTING Reaction mechanisms are investigate as a basis for models of aqueous metal-mineral transport processes 197. OXYGEN AND CATION DIFFUSION IN OXIDE applicable to a wide range of problems, from toxic metal MATERIALS migration in aquifers to scavenging of heavy metals $180,000 from solutions. Specific reactions to be investigated are DOE Contact: P. M. Davidson,(301) 903-5822 aqueous Cr(lll), Cr(VI), Cd(ll), Se(VI), Co(ll) solutions LLNL Contact: F. J. Ryerson, (510) 422-6170 with specified surfaces of representative phyllosilicates University of California at Los Angeles biotite, and chain silicates pyroxene and amphiboles. As Contact: K. D. McKeegan an outgrowth of this investigation, a widely applicable analytic tool is to be developed for measuring The objective of this work is to measure the diffusion Fe(ll)/Fe(lll) concentrations of small areas parameters for various cations and oxygen in important (approximately 25 x 50 microns) of silicates in thin rock-forming minerals to constrain both geochemical sections with X-ray photoelectron spectroscopy (XPS). transport processes and diffusive mechanisms affecting physical properties such as creep and electrical Keywords: Surface Reactions, High-Resolution conductivity. Oxygen self-diffusion coefficients have Transmission Electron Microscopy, been measured for three natural clinopyroxenes, a Phyllosilicates, Chain Silicates natural anorthite, a synthetic magnesium aluminate spinel, and a synthetic akermanite over oxygen 196. THE CRYSTAL CHEMISTRY AND fugacities ranging from the Ni-NiO to Fe-FeO buffers. STRUCTURAL ANALYSIS OF URANIUM OXIDE The oxygen self-diffusion coefficients of the three HYDRATES clinopyroxenes are indistinguishable. At a given $0 temperature, oxygen diffuses about 100 times more DOE Contact: P. M. Davidson, (301) 903-5822 slowly in diopside than indicated by previous bulk- University of New Mexico Contacts: D. Miller exchange experiments. New data for anorthite, spinel, and R.C. Ewing, (505) 277-4163 and akermanite agree well with prior results obtained by gas-solid exchange and depth profiling methods at Systematic crystal chemical relationships among different oxygen fugacities, indicating that diffusion of uranium oxide hydroxide phases which are initial oxygen in these nominally iron-free minerals is not corrosion products of uraninite ore and spent nuclear greatly affected by fO2 fuel, are investigated to help constrain systematic models for crystal structure topologies. Current work Keywords: Diffusion, Minerals, Plastic Deformation involves the determination of crystal structures for identified key missing phases, such as ianthinite and 198. STRUCTURE AND REACTIVITY OF FERRIC schoepite, which contain oxidized U6+ and are among OXIDE AND OXYHYDROXIDE SURFACES: corrosion products of UO 2 in near-surface, oxidizing QUANTUM CHEMISTRY AND MOLECULAR environments. Research objectives are to use the new DYNAMICS data on structural topologies to interpret and predict $200,000 speciation and thermodynamic stability relations among DOE Contact: P. M. Davidson, (301) 903-5822 uranium oxide hydrates. PNL Contacts: Jim Rustad and Andrew Felmy, (509)376-1134 Keywords: Uranium Oxide Hydrates, Crystal Chemistry Structural Topology The research is a theoretical investigation of the surface structure and reactivity of proton binding sites of ferric oxides and hydroxides. The surfaces of these common minerals are known to bind metals, oxy-anions, and organic chelates through mechanisms that are as yet poorly understood. The approach combines crystalline Hartree-Fock calculations for the ferric (hydr)oxides with a molecular dynamics (MD) model for water currently being developed by in collaboration with J. W. Halley of the University of Minnesota, in order to evaluate: (1) structures and relative stabilities of various ferric (hydr)oxide surfaces; (2) the most reactive sites for proton adsorption, indicated by relative proton affinities

95 Office of Energy Research in vacuo; (3) solvation corrections to relative surface temperature and pressure. The results provide much energies and relative proton binding energies; needed data on the nature of grain boundaries in rocks (4) improvements in thermodynamic models of proton and the rate of transport of chemical components adsorption resulting from better predictions of surface through rocks. Grain boundary diffusion of oxygen and structure, site types, and proton binding energies. cations in monominerallic aggregates of feldspar and of calcite, and aggregates of feldspar plus quartz were Keywords: Proton Adsorption, Surface Structure, determined with the ion microprobe (SIMS). Calcium Surface Reactivity, Ferric Oxides, Ferric grain boundary diffusion rates in Ca-rich feldspar Hydroxides aggregates are several orders of magnitude slower than oxygen, and than potassium in K-rich feldspar. This 199. CATION DIFFUSION RATES IN SELECTED suggests that differences in size and formal charge of MINERALS chemical species may play an important role in their $150,000 relative grain boundary diffusion rates. TEM analysis of DOE Contact: P. M. Davidson, (301) 903-5822 microstructures suggests that the equilibrium distribu- Sandia National Laboratory Contacts: tion of water in feldspar aggregates is that of isolated Randall T. Cygan, H. R: Westrich and Diana pockets. Studies continue in order to evaluate the role of Fisler, (505) 844-7216 pressure and nonhydrostatic stresses on fluid-feldspar interfacial energies and microstructures. Objectives of this research are to determine experimental cation diffusion coefficients for pyroxene Keywords: Diffusion, Rocks, Quartz, Feldspar, and carbonate minerals at temperatures less than Microstructures 1000°C for evaluating disequilibrium behavior in geological, nuclear waste, energy, and materials 201. THERMODYNAMICS OF MINERALS STABLE applications. A new thin-film technique for preparation NEAR THE EARTH'S SURFACE of diffusion couples was used to measure the relative $150,000 slow diffusion of Mg2*, Mn2' , and Ca2' in pyroxenes and DOE Contact: P. M. Davidson, (301) 903-5822 carbonates. Depth profiles of tracer isotopes are then UC Davis contact: A. Navrotsky, (916) 752-9307 evaluated using an ion microprobe. Comparison of the diffusion coefficients determined under various oxygen The objective of this research is to determine the fugacities provides information about the diffusion enthalpies of formation of hydrous minerals and mechanism and the defect structure of the mineral carbonates using high temperature solution calorimetry. sample. The experimental work has been Systematics in energetics of ionic substitutions are complemented by atomistic simulations of calcium sought in order to predict the thermodynamics of self-diffusion in calcite. Lattice energy, defect formation complex multicomponent minerals. Mixing properties of energies, and activation energy for a cation vacancy mica, amphibole, clay, zeolite, and carbonate solid migration have been calculated, providing the solutions are also analyzed. New calorimetric measure- mechanism and favored direction of migration of ments confirm significant differences in enthalpy cations in the calcite structure. Results suggest that between the ordered and disordered carbonate solution relaxation of atomic sites in the vicinity of a.cation series. Investigation of the energetics of ion exchange vacancy is a significant contribution to the energy for and hydration in zeolites is continuing, building on this the migration of cations. group's recently published solution enthalpies of a suite of Ca-zeolites and their ion-exchanged forms. Using Keywords: Cation Diffusion, Pyroxenes, Silicate drop solution calorimetry, the study of energetics of Minerals, Carbonate Minerals, Diffusion polytypism of the kaolin minerals has been extended to Mechanism, Defect Structure several differently crystallized kaolinites and the minerals nacrite and halloysite. Enthalpies of formation 200. GRAIN BOUNDARY TRANSPORT AND in the illite/smectite system have been measured for RELATED PROCESSES IN NATURAL FINE- the first time, providing good coverage of sedimentary GRAINED AGGREGATES sequences with different proportions of mixed layer $0 compounds. Measurements on natural illite/smectite DOE Contact: P. M. Davidson, (301) 903-5822 samples will be complemented with thermochemical Brown University Contacts: R.A Yund, measurements on selected synthetic compositional (401) 863-1931 and J.R. Farver series to address the effects of various levels of

The objective of this study is the direct measure of diffusional transport rates in rocks and how the rates vary with mineralogy and microstructure, as well as

96 Office of Energy Research impurities, and should provide constraints on the sulfides. Calculations have been completed on possible energetics of diagenetic processes. +2 oxidation state sulfur oxides and on surface relaxation in ZnS. Studies are in progress on the Hg Keywords: Thermochemistry, Solution Calorimetry, sulfides and some methyl-Hg species. Analysis of Zeolites, Carbonate Minerals, Clay aluminosilicate cage structures with single and double Minerals 4-ring geometries, is underway, with the goal of synthesizing new mineral-related compounds as 202. NEW METHOD FOR DETERMINING candidate flotation collectors with improved efficiency. THERMODYNAMIC PROPERTIES OF CARBONATE SOLID-SOLUTION MINERALS Keywords: Surface Complexation, Gold Sulfides, $133,661 Metal Transport DOE Contact: P.M. Davidson, (301) 803-5822 UC Davis Contacts: P.A. Rock and W.E. Casey, 204. MICROMECHANICS OF FAILURE IN BRITTLE (916) 752-0940 GEOMATERIALS $223,820 Incorporation of metals into calcium carbonate minerals DOE Contact: N.B. Woodward, (301) 903-5822 is an important pathway for elimination of potentially SUNY, Stony Brook Contact: Teng-Fong Wong, toxic metals from natural waters. The thermodynamic (516) 632-8240 properties of the resulting solution are, however, poorly SNL Contact: Joanne Fredrich (505) 846-0965 known because of difficulties with the solubility measurements. This project uses a new method of Differences in the onset of brittle failure in low-porosity measurement which avoids some of these difficulties. and high-porosity rocks depend on the cementation, The new method is an electrochemical double cell initial damage state and deformation history. However, including carbonates and no liquid junction. The cell is efforts to predict failure are hindered by the inability to an advance over conventional techniques because: (1) account for initial crack density and ductile intergranular reversibility can be directly established; (2) models of phases. For example, although cementation increases solute speciation are not required; (3) the brittle strength and reduces porosity, the toughening measurements do not perturb the chemistry mechanism is not well understood. This project aims to significantly. resolve this question with a systematic study of microstructures induced in experimentally deformed Keywords: Carbonate Minerals, Solubility, samples (both pre-and post-failure) of (1) high-porosity Electrochemical Cell carbonate rocks, in which plastic grain deformation and plastic pore collapse are thought to be important; (2) 203. THEORETICAL STUDIES OF METAL SPECIES sandstones of higher porosity but varying degree of IN SOLUTION AND ON MINERAL SURFACES cementation; (3) low-porosity crystalline rocks (as a test $55,817 of models on rocks with distinct mechanical properties). DOE Contact: P. M. Davidson,(301) 903-5822 University of Maryland Contact: John Tossell, Keywords: Brittle Failure, Plastic Deformation, (301) 314-1868 Experimental Rock Deformation, Cementation The project involves quantum mechanical (Hartree Fock) calculations of relative stabilities of species 205. THREE-DIMENSIONAL IMAGING OF DRILL participating in dissolution and precipitation of gold on CORE SAMPLES USING SYNCHROTRON- sulfide minerals. Although the solubility and surface COMPUTED MICROTOMOGRAPHY adsorption of aqueous Au species on sulfide minerals $225,000 are important agents of ore deposition, current DOE Contact: P. M. Davidson, (301) 903-5822 understanding is limited by lack of information on BNL Contact: Keith Jones, (516) 282-4588 surface complexation sites and speciation. This involves SUNY, Stony Brook Contact: W.B. Lindquist, the evaluation of structures, stabilities and spectral (516) 632-8361 properties of heavy metal sulfide species, such as As(SH)3 , Sb(SH)3 and Au(SH)2', both in aqueous Synchrotron radiation makes feasible the use of high solution and adsorbed on mineral surfaces and the resolution computed microtomography (CMT) for interaction of flotation collector molecules with sulfide non-destructive measurements of the structure of mineral surfaces. Predicted properties of As hydroxides different types of drill core samples. The goal of this provide a check for systematic comparison with work is to produce three-dimensional images of rock experimental data and with results for the corresponding drill core samples with spatial resolution of 1 micron.

97 Office of Energy Research

CMT images are postprocessed (filtered) to provide 207. DISSOLUTION RATES AND SURFACE specific grain/pore identification to each voxel in the CHEMISTRY OF FELDSPAR GLASS AND image. The pore topology is analyzed statistically to CRYSTAL yield information on disconnected pore volumes, throat $107,026 areas, pore connectivity and tortuosity. Current effort is DOE Contact: P. M. Davidson, (301) 903-5822 on development of software to analyze the Penn State Contact: S. Brantley, (814) 863-1739 3-dimensional connectivity and shape of the pore space using the medial axis theorem from computational Dissolution rates and mechanisms of the most common geometry. crustal mineral group, the feldspars, (Na,K,Ca) (AI,Si)AISi20g, are key factors in environmental Keywords: Synchrotron Radiation, Computed simulations of coupled fluid flow, effective water-rock Microtomography, Pore Structure, Drill surficial area, and fluid residence times. New dissolution Cores experiments and characterization of these silicate mineral and glass surfaces and solutions are underway 206. SHEAR STRAIN LOCALIZATION AND in order to help resolve discrepancies between existing FRACTURE EVOLUTION IN ROCKS laboratory measurements that are much faster than $144,987 dissolution rates observed in the field for feldspars in DOE Contact: N. B. Woodward, (301) 903-5822 soils, aquifers and small watersheds. Characterization Northwestern University Contact: J.W. Rudnicki, of the laboratory-reacted solids and naturally weathered (708) 491-3411 feldspars by IR and neutron methods for water content, and XPS and mass spectrometric methods for Prediction of the causative stresses, location, composition-depth profiling of leaching and surface orientation, thickness, and spacing of fractures in fault adsorption complemented with surface analysis by field- zones is important to energy production, waste emission SEM and AFM methods, will be used to disposal, and mineral technologies. This study constrain rate-controlling mechanisms of dissolution. examines the relation of fractures to the macroscopic Mechanistic information provided with a variety of constitutive description and microscale mechanisms of microanalytic methods that can encompass deformation by testing a standard theory of localization mechanisms of dissolution from glass to crystal and that describes faulting as an instability of the from laboratory to field environments will help to constitutive description of homogeneous deformation. A determine which of several competing dissolution new, more realistic nonlinear constitutive model, based models best describes the natural weathering process. on the growth and interaction of microcracks which produces increased bulk compliance, is being Keywords: Silicate Minerals, Dissolution Rates, developed and calibrated with axisymmetric Dissolution Mechanism, Surface Reactions, compression tests. Numerical studies (at SNL) will Surface Characterization evaluate the complications of realistic geometries and boundary conditions. Preliminary results suggest that 208. TRANSPORT PHENOMENA IN the response to an abrupt change in the pattern of FLUID-BEARING ROCKS deformation is completely nonlinear and cannot be $0 approximated accurately by incrementally linear DOE Contact: P. M. Davidson, (301) 903-5822 models, as is often done. This nonlinear response may Renssalaer Polytechnic Institute Contact: therefore be critical to the evolution of typical fault E.B. Watson, (518) 276-6475 zones. The research involves two parts: (1) determining the Keywords: Shear Strain Localization, Fracture solubility and diffusivity of selected rock-forming Evolution, Constitutive Description, minerals and mineral assemblages in deep C-O-H Nonlinear Behavior fluids, and (2) measuring the permeability of fluid-bearing synthetic rocks. A new procedure is being developed for measuring mineral solubilities and component diffusivities in fluids at pressures above 1 GPa, by measuring the total mass of transported component across a thermal gradient in dumbbell- shaped capsules at constant P (>1 GPa). Diffusivities are obtained from independent measurements of the component flux through different T gradients. In the second portion of the investigation, rocks synthesized at high (P > 1 GPa) pressures in the presence of differing

98 Office of Energy Research

fluid compositions and consequently porosity structure, OFFICE OF COMPUTATIONAL AND TECHNOLOGY will be analyzed at ambient conditions to determine RESEARCH permeability using dihedral angle measurements and bulk fluid (air) diffusion through the samples. Direct DIVISION OF ADVANCED ENERGY PROJECTS AND imaging of the pore structure will also be attempted with TECHNOLOGY RESEARCH Scanning Electron Microscopy and synchrotron X-ray tomography. LABORATORY TECHNOLOGY RESEARCH (LTR) PROGRAM Keywords: Diffusivity, Solubility, C-O-H Fluids, Porosity Structure, Rock Permeability The LTR program supports research primarily at the five ER multi-program national laboratories: Argonne, 209. CATION CHEMISORPTION AT OXIDE Brookhaven, Lawrence Berkeley, Oak Ridge and Pacific SURFACES AND OXIDE-WATER INTERFACES: Northwest. X-RAY SPECTROSCOPIC STUDIES AND MODELING The LTR program links advances in basic research at $246,861 the DOE laboratories to applied technologies of interest DOE Contact: P. M. Davidson, (301) 903-5822 to DOE mission areas through high-risk, multi- Stanford University Contacts: G. E. Brown, disciplinary research collaborations with private and G. A. Parks, (415) 723-9168 industry. The program funds the laboratories while the industry partners support their own participation at a This project concerns reactions and reaction level equal to the LTR funding. mechanisms between metal ions in aqueous solution and oxide surfaces representative of those found in the The LTR program builds upon the results of ER basic Earth's crust as an aid to developing both quantitative research and other DOE research programs in understanding of the geochemistry of mineral surfaces collaboration with industry partners to enhance mission- and the macroscopic models required to predict the oriented technologies at the laboratories while making fate of contaminants in earth surface environments. The technology available to industry for its use. The projects objectives of this research are (1) to characterize are selected in competitive peer reviews of solicited sorption reactions by determining composition, proposals submitted by the laboratories in conjunction molecular-scale structure, and bonding of the surface with their partners. complexes produced using direct sorption measurements, synchrotron-based X-ray absorption The following multi-year projects are supported by LTR fine structure (XAFS) spectroscopy, X-ray photoelectron at the five multi-disciplinary ER laboratories. spectroscopy (XPS), and UV/Vis/IR spectroscopy; (2) to investigate how these properties are affected by the MATERIALS PREPARATION, SYNTHESIS, solid surface, the composition of the aqueous solution, DEPOSITION, GROWTH OR FORMING the presence or simple organic ligands containing functional groups common in more complex humic and 210. LUMELOID, A NEW SOLAR ENERGY fulvic substances, and time; and (3) to develop CONVERSION MATERIAL (ANL94-42) molecular-level and macroscopic models of sorption $200,000 processes. DOE Contact: Walter M. Polansky, Keywords: Surface Complexation, Interace Reactions,L (301)Contact 903-5995 Michael Wasielewski, Chemistry ANL Contact: Michael Wasielewski, Chemistry, Synchrotron X-ray Absorption (630) 252-3538 Spectroscopy (630) 252-3538 The Argonne National Laboratory (ANL) is carrying out a research project to develop photoactive polymer composite materials to directly convert solar energy into electricity. This collaboration utilizes ANL expertise in developing photoactive materials in combination with ARDI film technology to generate new material

99 Office of Energy Research composites that could have a significant impact on 212. GIANT MAGNETORESISTANCE WIRE SENSOR cheap and efficient power generation from solar energy. (ANL95-07) $75,000 Keywords: Polymers, Composites, Solar Energy DOE Contact: Walter M. Polansky, Conversion (301) 903-5995 ANL Contact: Samuel Bader, Materials 211. COLD CATHODE ELECTRON EMISSION FROM Science, (630) 252-4960 DIAMOND AND DIAMOND-LIKE CARBON THIN FILMS FOR FLAT PANEL COMPUTER Giant magnetoresistance (GMR) materials are DISPLAYS (ANL95-02) composite metals whose resistance changes in the $140,000 presence of magnetic fields. These materials are up to DOE Contact: Walter M. Polansky, one hundred times more sensitive to magnetic fields (301) 903-5995 than previously known systems. Currently the GMR ANL Contact: Alan Krauss, MSD/CHM, materials are made by thin-film processing techniques (630) 252-3520 thereby making their cost prohibitive for many applications. The goal of this project is to develop giant Cold cathode electron emission has been observed magnetoresistance sensors by inexpensive bulk from a number of diamond and diamond-like carbon processing techniques such as wire drawing, and to thin films. It is expected that this phenomenon can be make prototype sensors that could be used in a variety used for the development of high visibility displays for of applications. critical applications such as avionics, high reliability microelectronics applications for operation in harsh Keywords: Composites, Electrical, Magnetics, Sensors environments where maintenance is not feasible, and flat panel computer displays. The development of 213. HIGH PERFORMANCE TAILORED MATERIALS devices like flat panel computer displays which use cold FOR LEVITATION AND PERMANENT cathode electron emission has been hampered by a MAGNETIC TECHNOLOGIES (ANL97-02) lack of basic understanding of the emission process. A $125,000 method has been developed at Argonne National DOE Contact: Walter M. Polansky, Laboratory for the growth of diamond films in the near- (301) 903-5995 absence of atomic hydrogen, using Ar-Co6 or Ar-CH4 ANL Contact: George W. Crabtree, Materials plasmas. This method produces films which respond Science, (630) 252-5509 differently to variations in growth conditions compared with films grown in large quantities of hydrogen. The The high temperature superconductor Nd,1 Ba2.,Cu307.y differences manifest themselves in the manner in which has recently been recognized as a powerful new the nucleation density, grain size, grain boundary width, material in which strong magnetic flux pinning has been surface roughness, crystallographic orientation and the observed. This material can be used for the develop- extent and localization of regions of sp2 and sp3 ment of levitators and trapped-field permanent magnets, electronic bonding character vary with the hydrogen creating an opportunity to drive substantial advances in concentration in the plasma. We have been able to the performance and technical competitiveness of these relate several of these properties to the effective work technologies. The development of this material will shift function, turn-on voltage and emission site density by the leading edge of materials research in this area from comparing the electron emission behavior and physical the two foreign laboratories (ISTEC, Japan and FZK, properties of conventional micro-and nano-crystalline, Germany) now dominating the field to the U.S. Although and low-hydrogen nanocrystalline diamond films. the strong pinning characteristics of this material have been recognized, the responsible pinning centers and Keywords: Diamond, Diamond-like, Coatings, Thin efficient procedures for large scale fabrication of the Films, Computer Displays material remain relatively obscure. ANL has identified a crucial new processing variable, the high temperature cooling rate during the growth process, which can be used to tailor the flux pinning properties of these materials. In addition, ANL has developed a low temperature oxygen anneal processing technique to control the magnetic field where maximum pinning occurs. An important objective of this project is to understand the origin of the superior flux trapping capabilities and to develop fabrication procedures using top-seeding techniques for making large samples for

100 Office of Energy Research

applications. Processing methodology will be developed suitable membrane materials at ANL, and the based on property measurements using X-ray and construction of a prototype reactor to evaluate the neutron diffraction, magneto-optical imaging, materials performance and demonstrate the viability of magnetization measurements, and scanning tunneling the process at Amoco. A suitable ceramic membrane microscopy on melt-textured material and single crystal material, that demonstrates the potential for the desired samples. The best material will be tested in prototype performance, has been developed in previous work. levitating flywheels to assess its value and define However, the exact chemical composition and crystal problem areas in collaboration with our industrial structure of this material is not known. Neutron and partner, Superconductive Components, Inc. The x-ray diffraction techniques will be used to determine development of high performance flux pinning materials this information. This will allow the synthesis and will enable a new generation of levitation devices for processing of the membrane material to be optimized to frictionless bearings and flywheel energy storage, and of produce the best performance. in situ neutron diffraction permanent trapped-field magnets. The materials at elevated temperature in conditions that simulate the performance advances achieved under this project can environment in a working syngas reactor will be used to be applied to other developing technologies, such as study aspects of the materials related to achieving the coated conductors for high current carrying wires (IBAD longest possible working lifetime. Existing laboratory and RABITS), and high power microwave filters for and pilot plant facilities will be upgraded and modified to cellular communications. (1) The emission sites will be facilitate testing of the ceramic membranes under identified, and a determination of the site density will be increasingly rigorous conditions. This will provide a made, using photo-electron emission microscopy valid test of the suitability of the ceramic materials for (PEEM) for several varieties of electron emitting use in large-scale reactors that convert natural gas into diamond and diamond-like carbon films. The project syngas and, at the same time, a useful test of the team has found that post-deposition treatment is critical overall process. in controlling emission properties, and the PEEM data will be studied in conjunction with oxygen and hydrogen Keywords: Natural Gas, Synthesis Gas (syngas), plasma post-deposition processing. (2) Studies of the Ceramic Membranes, Testing of grain morphology of films produced both at SI Diamond Membranes, Oxygen-Permeable and at ANL are being conducted using transmission Membranes electron microscopy. The ANL portion of these tasks will continue with funding from the Advanced Projects 215. COMPOSITE METAL-HYDROGEN Research Agency as part of a program for improvement ELECTRODES FOR METAL-HYDROGEN of diamond cathode materials for high resolution BATTERIES (BNL94-06) displays. Research in diamond structures and $115,000 applications to electronics support DOE's long standing DOE Contact: Walter M. Polansky, mission in materials sciences. (301) 903-5995 BNL Contact: Myron Strongin, Physics Keywords: Superconductors, Permanent Magnets, Department, (516) 344-3763 Processing Techniques, Materials Performance The project focuses on the fabrication and characterization of nano-scale bimetallic multilayered films and 214. SYNTHESIS AND CRYSTAL CHEMISTRY OF a feasibility study of their use as hydrogen-containing TECHNOLOGICALLY IMPORTANT CERAMIC negative electrodes (anodes) in nickel-metal hydride MEMBRANES (ANL97-06) (NiMH) batteries. If the feasibility of using these new $125,000 materials is established, it is anticipated that the project DOE Contact: Walter M. Polansky, will contribute to the advancement of NiMH battery (301) 903-5995 technology and provide batteries with more rapid ANL Contact: James D. Jorgensen, Materials charging characteristics, greater energy efficiency or Science Division, (630) 252-5513 larger energy storage capacity.

Achieving the conversion of natural gas.to synthesis gas Keywords: Composite Electrodes, Metal-Hydrogen (syngas) using oxygen-permeable ceramic membranes Electrodes, Batteries would bring vast resources of natural gas within our economic reach. This new technology depends on the development of suitable ceramic membrane materials whose performance is then demonstrated in prototype reactors. This project includes the development of

101 Office of Energy Research

216. DEVELOPMENT OF CdTe/CdZnTe MATERIALS and the role of the individual alloying additions. FOR RADIATION DETECTORS Ultimately an understanding of the interactions between (BNL94-09) alloy composition and the electrochemical response of $115,000 alloys with optimum mechanical properties and DOE Contact: Walter M. Polansky, biocompatibility will be developed. in situ XANES (301) 903-5995 measurements in simulated bio-fluid (Ringer's solution) BNL Contact: Csaba Szeles, Physics, and under crevice conditions (concentrated chloride (516) 344-3710 solution) will provide information on the chemical behavior of the alloys during corrosion. A detailed study The objective of this project is to broaden the potential of oxide formation will be carried out using XANES, use of Cadmium Zinc Telluride (CdZnTe) materials as surface analytical techniques and in situ AFM. room-temperature solid-state radiation detectors. Achieving this goal requires improvement of the existing Keywords: Corrosion Resistance, Biomedical, material-growth and processing techniques in order to Applications, Alloys enhance the production yield and energy resolution of CdZnTe crystals limited by the unpredictability of the 218. CATALYTIC PRODUCTION OF ORGANIC as-grown material. This unpredictability is largely due to CHEMICALS BASED ON NEW the uncontrolled incorporation of electrically active HOMOGENEOUSLY CATALYZED IONIC native and impurity-related defects in the bulk and at the HYDROGENATION TECHNOLOGY surface of the crystals and defects at the (BNL97-05) semiconductor-metal interface. Production of better $118,000 crystals demands improved understanding of the nature DOE Contact: Walter M. Polansky, of lattice defects, their influence on the detector (301) 903-5995 performance and their formation and compensation BNL Contact: Morris Bullock, Chemistry mechanism during the crystal growth and processing. Division, (516) 344-4315 The availability of inexpensive, high-efficiency, room- temperature gamma-ray detectors is of great This project will focus on the development of new commercialization potential. It stimulates instrument technology for the production of organic chemicals of and device manufacturers to develop new products and commercial interest, based on fundamental research at retrofit old applications using conventional Nal(TI) and BNL exploring the reactivity of transition metal hydride HPGe detectors. The total addressable market for complexes. The scientific objectives are to explore the CdZnTe materials and the new instruments and devices feasibility, scope, and selectivity of catalytic ionic that integrate CdZnTe as a primary gamma-ray detector hydrogenation technology. In these reactions, H2 is is in excess of 40 million dollars annually. DOE has added to an organic chemical sequentially, in the form extensive programs which use X-ray, gamma-ray and of a proton (H+) followed by hydride (H-). The project particle detectors. Improved, low-cost, room- plans to discover transition metal complexes that can temperature radiation detectors are important for a carry out these functions catalytically, with hydrogen number of key DOE programs such as nuclear safety (H2) being the ultimate source of both the proton and and safeguards, field assays, X-ray and gamma- hydride. Homogeneously catalyzed ionic hydro- detectors for next generation light sources, solar cells, genations offer the possibility of enabling efficient and X-ray and gamma-ray satellite surveillance etc. selective hydrogenation processes for organic transformations that are difficult to achieve by Keywords: CdZnTe, Radiation, X-ray, Gamma conventional methods. Initial work will focus on Detectors attempts to develop prototype metal systems capable of catalytic hydrogenation of ketones. Tungsten systems 217. CORROSION RESISTANCE OF NEW ALLOYS with weakly coordinating counterions will be investi- FOR BIOMEDICAL APPLICATIONS (BNL94-20) gated first, since preliminary results have indicated that $140,000 such systems have the requisite ability to form cationic DOE Contact: Walter M. Polansky, tungsten dihydride complexes upon reaction with H2. A (301) 903-5995 key issue to be addressed will be the relative binding BNL Contact: Hugh Isaacs, Applied Science, strength of different ligands to the metal, and measure- (516) 344-4516 ments of this type may require high pressure nuclear magnetic resonance experiments at DuPont. When a The development of new materials for prosthetic successfully functioning catalytic system is developed, devices and other biomedical applications is currently optimization will be attempted by systematic variation of underway. The objective of this project is to provide a ligands and the metal. Further elaborations will later detailed understanding of alloy corrosion in bio-systems attempt to utilize these methods in asymmetric

102 Office of Energy Research

hydrogenations to produce commercially viable 220. ALLOY DESIGN OF NEODYMIUM (Nd2FeO4B) processes. This project supports the fundamental DOE PERMANENT MAGNETS (ORL94-15) mission in understanding the mechanisms for catalysis $155,000 and the chemical conversion of materials from biomass. DOE Contact: Walter M. Polansky, (301) 903-5995 Keywords: Catalytic Production, Ionic Hydrogenation, ORNL Contact: Joseph Horton, Metals and Hydrogen, Organic Transformations, Ceramics, (423) 574-5575 Catalysis The objective of this project is to improve the room 219. NOVEL BIOCOMPATIBLE "SMART" CONTACT temperature fracture toughness of the neodymium LENS MATERIAL (LBL94-28) permanent magnet without decreasing its magnetic $211,000 properties. This will improve machinability, allow closer DOE Contact: Walter M. Polansky, tolerances, use as a structural element and more rapid (301) 903-5995 and further market penetration for uses such as electric LBNL Contact: Carolyn Bertozi, Materials motors. Sciences Division, (510) 643-1682 Keywords: Neodymium Magnets, Alloy Design, Vision is by far the most important of the human senses Fracture Toughness, Electric Motors and better ophthalmological care products are continuously being sought. For example, current 221. DEVELOPMENT OF ALUMINUM BRIDGE DECK synthetic contact lens materials have limited tolerance SYSTEM (ORL94-56) by the population. The project goal is to develop $105,000 improved materials that will increase the quality of life DOE Contact: Walter M. Polansky, not only for current wearers but also for those whose (301) 903-5995 physiology cannot tolerate existing materials. In our ORNL Contact: H. Wayne Hayden, Metals & design of new contact lens materials, we utilize the Ceramics, (423) 574-6936 lessons we have learned in nature. Our approach is to modify materials with favorable lens properties so that The purpose of this project is to investigate refinement they more closely resemble biological tissue, and are of the aluminum bridge deck panel system using therefore tolerated well by the eye. The knowledge aluminum multi-void extrusions joined together to make gained here is expected to further the understanding of panel sections. The desired results could be of use for how materials behave in a physiological environment the upgrading of deficient bridges throughout the U.S. and benefit biomedical implant devices development in with the use of aluminum bridge decks, and to use general. The work represents a significant advance in aluminum decks on new bridges. the development of new biocompatible materials. The first phase in the development of new contact lens Keywords: Aluminum Bridge Decks, Cost Effective, materials is the design of biocompatible monomers.for Lightweight Systems, Consortium incorporation into hydrogel polymers. In order to create lenses that best mimic biological tissue, we focused on 222. MANUFACTURING OF Ni-BASE carbohydrate molecules which comprise the coating of SUPERALLOYS WITH IMPROVED HIGH- most living cells. Our strategy, therefore, is to TEMPERATURE PERFORMANCE (ORL95-05) synthesize polymerizable monomers possessing cell $137,000 surface-like carbohydrates, and to incorporate them into DOE Contact: Walter M. Polansky, lenses with better biocompatibility properties. (301) 903-5995 ORNL Contact: C. Liu, Metals and Ceramics Keywords: Biocompatible, Smart Contact Lens, Division, (423) 574-4459 Materials, Monomers, Hydrogel Polymers The objective of this research project is to enhance the manufacturing of high-temperature nickel-base superalloys with improved performance through the control of vital minor elements in the parts-per-million range without significantly increasing production cost. It is anticipated that the control of these vital elements would extend the creep rupture life of superalloy structural members by more than an order of magnitude. Nickel-base superalloys are state-of-the-art

103 Office of Energy Research

materials for high-temperature structural applications in (4) thin film battery structures utilizing polymer-only advanced engines, petrochemical, other energy electrolyte layers. conversion systems. Keywords: Polymer Multilayer Films, Optics, Keywords: Ni-base Superalloys, High-Temperatures, Electrolytes and Glazings, Film Deposition Manufacturing 225. DEVELOPMENT OF MIXED METAL OXIDES 223. NEW THERMOELECTRIC MATERIALS FOR (PNL94-28) SOLID STATE REFRIGERATION (ORL95-10) $25,000 $150,000 DOE Contact: Walter M. Polansky, DOE Contact: Walter M. Polansky, (301) 903-5995 (301) 903-5995 PNNL Contact: Larry Pederson, Materials and ORNL Contact: Brian Sales, Solid State Chemical Sciences, (509) 375-2731 Division, (423) 576-7646 This research is directed towards the development of The goal of this project is to develop new materials that unique lithiated metal oxides for use in secondary will significantly improve the performance of thermo- batteries. The oxides will be produced using PNNL's electric devices for solid state refrigeration and air glycine nitrate process and will involve varying the conditioning. Thermoelectric refrigerators involve no compositions of the materials to optimize their desired moving parts, use no greenhouse gases, and are properties. Lithiated manganese oxides are expected to extremely reliable. ORNL will synthesize candidate be used in future lithium ion systems and a lithium thermoelectric materials along several paths including polymer system (which is becoming commercially filled and unfilled materials with the skutterudite available with a vanadium oxide cathode). The lithium structure and unusual "kondo-like" alloys, polymer system is expected to be used as a power source for electric vehicles later in this decade. Keywords: Thermoelectric Devices, Refrigeration, Air Conditioning, Alloys Keywords: Mixed Metal Oxides, Lithiated Metal Oxides, Lithiated Mn Oxides, Secondary 224. POLYMER MULTILAYER (PML) FILM Batteries, Polymer Systems APPLICATIONS IN OPTICS, ELECTROLYTES, AND GLAZINGS (PNL94-06) 226. DEVELOPMENT OF TAPE CALENDARING $200,000 TECHNOLOGY FOR SEPARATION DOE Contact: Walter M. Polansky, MEMBRANES (PNL95-04) (301) 903-5995 $257,000 PNNL Contact: John Affinito, Materials and DOE Contact: Walter M. Polansky, Chemical Sciences, (509) 375-6942 (301) 903-5995 PNNL Contact: Timothy Armstrong, Materials & The work undertaken in this research is in response to Chemical Sciences, (509) 375-3938 the requirement of a number of industries for a much higher rate, and much lower cost, process for vacuum The purpose of this research is to develop tape deposition of dielectric and/or deposition techniques. calendering technology to produce mixed conducting The Polymer Multi-Layer (PML) deposition technology and oxygen ionically conducting oxide membranes for being developed at PNNL, can deposit fully cured use as air separation and oxygen production devices. polymer films, in a roll-to-roll web coating system, at Tape calendering technology shows exceptional line speeds in excess of 600 linear meters per minute. promise as a means to manufacture complex ceramic While the technology developed under this research can structures on a large scale and at low cost. This project potentially be applied in many applications, in this could provide key technology that would help to produce project, four application areas are being explored. These large quantities of oxygen at a significantly lower cost are: (1) deposition, on flexible polyester substrate, of: than current cryogenic methods. Tape calendering enhanced and protected polymer/Ag/ polymer and combines oxide powders, binder, and plasticizer in a polymer/A/ polymer reflectors; (2) all polymer high-intensity mixer. The binder-plasticizer system can (polymeri/ polymer2)N, Quarter Wave Optical be softened by externally heating the mixing chamber, Thickness (QWOT) multilayer reflection filters; using only internal heating resulting from frictional (3) polymer/ silver/polymer 'Heat Mirror" structures; and forces generated within the mixing chamber, or combinations of the two. The softened binder system mixes with the ceramic powder to form a plastic-like mass. The mass is calendered into a thin, flat tape

104 Office of Energy Research using a two-roll mill with counter rotating rolls. Tape the biologically relevant calcium oxalate, carbonate, and thickness is controlled by the spacing of the two rolls. phosphate systems will be developed. Biological polymers of human serum albumin, Protein G, and Keywords: Tape Calendering of Oxide Membranes, fibrinogen will be used in the adsorption experiments. Separation Membranes, Air Separation, These provide excellent models since they exhibit a Oxygen Production, Complex Ceramic range of structures, sizes, and chemistries. State of the Structures art techniques of neutron scattering and reflectometry, quartz crystal microbalance, liquid chromatography/ 227. INNOVATIVE MULTILAYER THERMAL mass spectroscopy, and atomic force microscopy will BARRIER COATINGS FOR GAS TURBINE be employed to study adsorption in situ. Information on ENGINES (PNL95-07) adsorption kinetics, isotherms, and protein $245,000 conformation will be obtained in real time. Finally, solid DOE Contact: Walter M. Polansky, state nuclear magnetic resonance experiments will be (301) 903-5995 conducted to identify the specific protein residues that PNNL Contact: Edward Courtright, Materials & are interacting with the surface. This investigation will Chemical Sciences, (509) 375-6926 provide molecular level information on specific interactions that has not yet been obtained. The project The objective of this project is to determine the will contribute to achieving DOE's mission in feasibility of producing innovative multilayer thermal fundamental science, while also providing knowledge barrier coatings. The fundamental issues associated and technology to potentially enable the development of with maximizing infrared reflectivity and phonon improved materials for use in health care. scattering, and the thermodynamic stability issues which affect durability, reliability, and life-cycle perfor- Keywords: Interfacial Interactions, Biological mance are being investigated. In the first phase of the Polymers, Model Surfaces, Design program, the feasibility of producing higher performance Synthesis and Characterization, Vapor thermal barrier coatings with multilayered systems will Deposition be demonstrated. In the second phase of the program, actual components will be coated and tested under 229. HIGHLY DISPERSED SOLID ACID CATALYSTS simulated engine conditions, e.g., burner rigs or in ON MESOPOROUS SILICA (PNL97-28) actual land-based gas turbine engines $125,000 DOE Contact: Walter M. Polansky, Keywords: Thermal Barrier Coatings, Multilayer (301) 903-5995 Coatings, Gas Turbine Engines, Thermal PNNL Contact: Yong Wang, (509) 376-5117 Barriers This project will develop new materials optimized for 228. INTERFACIAL INTERACTIONS OF use as solid acid catalysts by coupling the advanced BIOLOGICAL POLYMERS WITH MODEL characteristics of mesoporous silica with the SURFACES (PNL97-21) superacidic properties of tungstophosphoric acid and $124,000 sulfated zirconia. The surface of mesoporous silica will DOE Contact: Walter M. Polansky be functionalized to accommodate the dispersion of (301) 903-5995 tungstophosphoric acid and sulfated zirconia. This PNNL Contact: Allison Campbell, Materials and approach should produce a new class of highly active, Chemical Sciences Division, (509) 375-2180 shape selective, and robust solid superacid materials. The novel catalysts will be tested with the alkylation and The adsorption of biological polymers onto surfaces isomerization reactions in the bench and pilot scale affects many different industrial processes. However, testing unit. The goal is to exceed the performance the controlling mechanisms and the interfacial structure characteristics of existing solid superacid catalysts, are not well understood for most systems. This project thereby enabling the chemical and petrochemical will develop and apply state of the art methods to industries to replace homogeneous acid catalysts. This design, synthesize, and characterize systems for will contribute to DOE's mission to reduce environ- adsorption experiments. Specifically, molecular beam mental impacts in the energy sector. Homogeneous epitaxy, chemical vapor deposition, and self-assembling acid catalysts such as sulfuric acid and aluminum monolayers will be used to construct surfaces with chloride are currently used to catalyze many of controlled properties such as chemistry, topography, industrially important reactions. Although these and heterogeneity. For the first time, chemical vapor homogeneous acid catalysts are efficient, they are not deposition methods for producing controlled surfaces of environmentally benign and create many operational

105 Office of Energy Research problems. These problems can be mitigated with solid its current suite of state-of-the-art computational tools. acid catalysts. Tungstophosphoric acid and sulfated This new capability can then be used for other DOE zirconia are two solid acid catalysts with super acidity. projects that require modeling of composite materials. Low catalytic efficiency is the common problem with these two catalysts. In addition, it is difficult to disperse Keywords: Composites, Modeling, Analyses tungstophorsphoric acid on supports due to its large cluster size and sulfated zirconia generally suffers rapid 231. DEVELOPMENT OF RAPID PROTOTYPING deactivation. These problems can be minimized with the TECHNOLOGY FOR BIOCERAMIC superior characteristics of mesoporous silica. This work APPLICATIONS, (ANL 95-08) will enhance understanding of how the mesoporous $276,000 support properties and acid grafting strategy influence DOE Contact: Walter M. Polansky, reactivity, yields, selectivity, thermal stability, coking, (301) 903-5995 and regeneration of the solid acid catalysts. Research ANL Contact: William A Ellingson, Energy under this project was initiated in August 1997. To date, Technology Division, (630) 252-5068 efforts have been conducted to define the specific catalyst properties of interest. Initial synthesis and This project addresses the need to reduce medical costs functionalization of the mesoporous silica supports has associated with orthopaedic implant design, fabrication, also been initiated. and implantation, including medical costs for injury recovery time, as many situations require special Keywords: Solid Acid Catalyst, Mesoporous Silica, implant configurations and designs. The approach is to Tungstophosphoric Acid, Sulfated Zirconia reduce the cost of producing these complex implants using FDA approved bio-ceramic materials through two DEVICE OR COMPONENT FABRICATION, activities: (1) development of a new fabrication BEHAVIOR OR TESTING technology called "Rapid Prototyping" (also called Solid Freeform Fabrication) through use of FDA approved 230. APPLICATION OF HIGH PERFORMANCE bioceramic materials, and (2) development of reverse COMPUTING OF AUTOMOTIVE DESIGN AND engineering technology using 3-Dimensional X-ray MANUFACTURING (ANL94-54) Computed Tomographic Imaging (often called CAT $175,000 scans in the press) and necessary advanced digital DOE Contact: Walter M. Polansky, imaging methods. Tasks in the project include (301) 903-5995 development of: (1) appropriate bioceramic feed stock ANL Contact: David Weber, Reactor for the rapid prototyping machine, (2) binder bum out Engineering Division, (630) 252-8175 and sintering schedules for the bioceramic materials, (3) machine parameters for proper fabrication of these This research focuses on the application of high- materials, (4) digital image methods to allow digital files performance computing to automotive design and to be extracted from the "CAT" scan images to allow manufacturing. The major thrust of the work is to use by the rapid prototyping machine, (5) algorithms to develop easy-to-use computer codes for new high allow digital image files as input to CAD software performance computing (HPC) platforms. Argonne packages for design modifications, and (6) surgical National Laboratory is focusing on two areas: implant procedures for these new implants. To date, computational fluid dynamics and composite material selected bones (chosen by the industrial partners as modeling. The Computational Fluid Dynamics (CFD) being of importance), hand and forearm, have been task will develop "next generation" computational tools used for high resolution X-ray imaging, and digital for the analysis of CFD phenomena. These tools, images have been obtained. The files have been including improved physical models and taking extracted and modified to allow input to the rapid advantage of advanced parallel computing architec- prototyping machine. (Feedstock materials for the rapid tures, will allow manufacturers to design improved prototyping machine, using aluminum oxide, have been systems and shorten the design time. The Composite developed including binder burn out and sintering Materials Modeling Task will develop predictive schedules.) The first hand bone and forearm bone have numerical analysis tools. This research will: (1) permit been fabricated using the feedstock material and the the reliable incorporation of lightweight fiberglass rapid prototyping machine. New bioceramic materials reinforced composites into the design of more fuel including hydroxyapetite/tricalciumphosphate are now efficient passenger automobiles without compromising under development. Machine parameters, including passenger safety, (2) decrease design and manu- thickness of layer, filament temperature, and facturing times and cost, and (3) result in a decrease in cross-head speed, have been established for using the domestic fuel consumption. DOE will benefit by adding new feedstock material. The reverse engineering advanced numerical methods for composite materials to research is currently under study by the industrial

106 Office of Energy Research partner for application. This project supports the DOE research developments in material sciences to mission in materials research and medical applications, improved processing technologies.

Keywords: Rapid Prototyping, Bioceramics, Keywords: Diamonds, Films, Coatings, Applications Applications, Reverse Engineering, CAT Scans, Bones, CAD 233. MICROFABRICATION OF A MULTI-AXIS MICRO-ACCELEROMETER USING HIGH 232. SMOOTH DIAMOND FILMS FOR FRICTION ASPECT RATIO MICROFABRICATION (HARM) AND WEAR APPLICATIONS AND CHEMICALLY AND SILICON MICROMACHINING (BNL94-02) PROTECTIVE COATINGS (ANL97-05) $100,000 $150,000 DOE Contact: Walter M. Polansky, DOE Contact: Walter M. Polansky, (301) 903-5995 (301) 903-5995 BNL Contact: John Warren, Instrumentation, ANL Contact: Alan R. Krauss, D. M. Gruen, (516) 344-4203 Materials Science and Chemistry Division, (630) 252-3520 The primary goal of this project is to use high aspect ratio microfabrication to bulk fabricate all of the Diamond has a number of properties which, in principle, components of a multi-axis accelerometer. The inherent make it an exceptional material for a large number of accuracy of the microfabrication process (based on applications. In particular, the extreme hardness (harder lithography) should also lead to improvements in than any other known material), chemical inertness (it performance. The completed micro-accelerometer will resists attack by almost all known acids and bases), have many applications in aviation, auto navigation, and low coefficient of friction (comparable with that of active automotive suspension system control, drill bit TeflonT") make it an ideal candidate for a wide range of navigation, and airbag deployment. The high aspect applications involving sliding or rolling contact between ratio microfabrication process has many scientific moving surfaces. However, conventional diamond applications and is currently being used in the chemical vapor deposition (CVD) methods produce Instrumentation Division at BNL to construct prototype coatings with extremely rough surfaces. This roughness position-sensitive X-ray detector arrays that have many has limited the development of diamond film technology applications in high energy physics. Knowledge gained for tribological applications, and penetration of diamond from microfabrication methods is directly applicable to film technology into these markets has been these on-going efforts. disappointingly slow. This project concerns the use of a process developed at Argonne National Laboratory for Keywords: Microfabrication, Accelerometer, X-ray the production of ultra-smooth diamond coatings on Detector rotating and sliding mechanical parts in order to reduce energy consumption, improve product reliability, and 234. NONDESTRUCTIVE X-RAY SCATTERING reduce toxic emissions into the environment. Films CHARACTERIZATION OF HIGH produced by this process have been shown to possess TEMPERATURE SUPERCONDUCTING WIRES tribological properties which eliminate the problems (BNL95-10) which have so far limited the use of diamond coatings $160,000 for applications involving moving parts. The work to be DOE Contact: Walter M. Polansky, performed addresses adaptation of the process for the (301) 903-5995 production of diamond coatings that are 10-100 times BNL Contact: Thomas Thurston, Physics, smoother than those produced by existing processes. (516) 344-5534 End face mechanical seals, used to prevent the leakage of gases and liquids in equipment with rotating shafts, Prototypes of generators, transformers, transmission have been chosen as the area of application. The cables, and current limiters which utilize wires made of benefits obtained in terms of energy savings, increased high-temperature superconducting materials are just productivity, reduced maintenance, and reduced release beginning to be built. Although the ultimate purposes of of environmentally hazardous materials for this single these electric power devices vary, all of them offer the application will be substantial, but the technology which potential for substantial energy savings, since there is will be developed will also be directly applicable to a. no loss of energy in the form of heat generated by large number of application areas in manufacturing and electrical resistance. DOE has programs to develop transportation, in most cases with similar benefits. This technologies for electric power applications of high project supports DOE mission in the application of basic temperature superconductors. All of the electric power applications of high-temperature superconductors

107 Office of Energy Research described above require long lengths (at least a new low cost polymer electrolyte, with good -100 meters) of wire with large current carrying conductivity, and excellent adhesion to the electrodes. capacities. Unfortunately, there are a variety of effects that can limit the current carrying capacity of the wires, Keywords: Thin Films, Lithium, Batteries with the consequence that today's wires have capacities which are at least 10 times smaller than the maximum 236. NEW CATALYSTS FOR DIRECT METHANOL theoretical capacity. The purpose of this research is to OXIDATION FUEL CELLS (BNL95-14) characterize the structure of the superconducting $80,000 material within wires in order to understand the causes DOE Contact: Walter M. Polansky, of poor current carrying capacity, and to suggest (301) 903-5995 alternative processing procedures which can minimize BNL Contact: Radoslav Adzic, Applied or eliminate the effects which cause poor wire Science, (516) 344-4522 performance. The methods which Brookhaven is using to characterize the wires utilize intense beams of X-rays A search for an active metal oxide-metal electro- generated at Brookhaven's National Synchrotron Light catalysts for methanol oxidation has been performed Source. Work performed earlier showed that the current with platinum electrocatalyst supported on several types carrying capacity is affected by the presence of certain of metal oxides. Synthesis and the electrochemical impurity phases, and by poor texturing of the and/or spectroscopic characterizations were carried out. superconducting material within the wires. Both of these A very active electrocatalyst was obtained with Pt deleterious effects can be readily measured only with supported on Ru oxide. Reaction intermediates and the intense X-ray beams available at facilities like the products for some systems were characterized by in situ National Synchrotron Light Source. Work currently in Transform Infrared Spectroscopy (FTIR). progress involves direct X-ray monitoring of superconducting wire processing in a "mini-factory" Keywords: Electrocatalysts, Methanol Oxidation, Fuels which has been set up at Brookhaven. This work has Cells already suggested modifications increase the current carrying capacity of wires. BNL has started to apply the 237. DEVELOPMENT OF MULTI-CHANNEL ASICs techniques developed to characterize these wires on FOR CdZnTe GAMMA DETECTOR ARRAYS other problems of interest to the DOE, such as (BNL97-06) characterizing the properties of battery electrode $82,000 materials and permanent magnets. DOE Contact: Walter M. Polansky, (301) 903-5995 Keywords: Superconducting Wires, Prototypes, BNL Contact: Paul O'Connor, Instrumentation Characterization, High-Temperature Division, (516) 344-7577

235. THIN FILM LITHIUM BATTERIES, (BNL95-11) The objective of this project is to develop an X-ray $80,000 imaging module consisting of a multi-element Cadmium DOE Contact: Walter M. Polansky, Zinc Telluride (CZT) detector and a CMOS application- (301) 903-5995 specific integrated circuit (ASIC). The module will detect BNL Contact: James McBreen, Applied x and gamma rays in the energy range from 20 - 150 Science, (516) 344-4513 keV in the photon counting mode. The electronics must be compatible with the CZT detector characteristics and This research is focused on the development and at a minimum preamplify and shape the pulse signals testing of polymer electrolytes for primary thin film from the detector elements. There is currently a large lithium batteries. A cell design, based on thin need for solid state gamma and X-ray imaging electrodes, with the cell enclosed in a thin heat sealed capability for both medical and industrial applications. foil-laminate pouch like that used in the food industry In industry, a need exists for imaging food products for (e.g., coffee) has been developed by an industry source. foreign matter, non-contact, high speed weighing of While this design is attractive for thin film batteries, and consumer products to ensure minimum weight is adequate for prevention of ingress of water vapor or compliance and multi-energy high speed imaging of air, it presents many technical challenges. The foil manufactured products to detect subtle defects. Solid laminate gives no mechanical support to ensure state CZT arrays offer the possibility of reducing the intimate contact between the electrodes and the weight and bulkiness of existing nuclear medicine electrolyte. Bulging of the pouch and its contents can cameras based on Nal scintillators and photomultiplier result in large increases in the resistance losses in the angular camera technology. Small hand held imaging cell. These problems were solved by the development of devices show promise for locating cancer tissue during surgery through the use of monoclonal antibodies

108 Office of Energy Research tagged with radioactive tracers. For security screening, range, linearity, crosstalk, and power consumption) will CZT arrays when used with multi-energy X-rays can first be specified based on a knowledge of the 2D bar detect explosives and other contraband. The technical code reader system. We plan to model alternative approach consists of the evaluation of the performance photodetectors using the semiconductor device of various existing BNL circuits with CZT arrays, simulation codes currently used at BNL for silicon adapting the existing design so that the front end and radiation detector development. This project supports shaping parameters are ideally matched to the CZT the DOE mission in advanced semiconductor research detectors, producing a prototype array of a certain size for development of crosscutting sensor technologies. by tiling arrays and ASIC circuits, developing a 64 or greater channel ASIC for larger substrates (or finer Keywords: Data Collection and Transmissions, CMOS pitch), and configuring existing building blocks to build a Process, Integrated Circuits, Microcircuits, multiplexing and image processing ASIC. The Sensors, Imaging Arrays development of these solid-state detectors will benefit DOE mission areas in time-resolved X-ray 239. RECHARGEABLE ZINC/AIR BATTERIES FOR crystallography, nuclear medicine, and extended X-ray CONSUMER APPLICATIONS (LBL94-43) absorption. $62,000 DOE Contact: Walter M. Polansky, Keywords: ASICs, CdZnTe Detector Arrays, (301) 903-5995 Application, Solid State Detectors LBNL Contact: Elton Cairns, Energy 8 Environment Division, (510) 486-5028 238. MICROCIRCUITS AND SENSORS FOR PORTABLE, LOW-POWER DATA COLLECTION The Zn/air battery is an especially appealing technology AND TRANSMISSION (BNL97-07) for use in consumer batteries because of its high $125,000 specific energy, low cost and environmentally benign DOE Contact: Walter M. Polansky, components. The zinc-air technology is greatly under- (301) 903-5995 utilized because of the generally low power available BNL Contact: Paul O'Connor, Instrumentation from the cell. The power limitations stem primarily from Division, (516) 344-7577 the air electrode as a result of the slow kinetics of the electrochemical reduction of oxygen from air. Complete The objective of this project is to design, fabricate and utilization of the zinc loading can also be a problem at test two novel devices for data collection and high power drains. The focus of this project has been to transmission: an optical photosensor array and a address these two limitations in order to extend the 2.4 GHz, single-chip, frequency-agile radio transceiver. possible markets for the zinc/air primary battery Both devices can be processed in a standard CMOS technology. The first year of this project has been integrated circuit process. CMOS technology has concerned with the application of novel electrocatalysts advanced to the point where many conventional to the air electrode structure to improve the high-power electronics systems can be fully integrated on a single performance of this electrode. The second year will chip. Up to now the vast majority of these chips perform focus on the study and modification of the zinc purely electronic functions. In this project we propose to electrode formulation in order to optimize zinc utilization investigate two integrated circuits with sensors which at high power. Four electrocatalyst systems are under can process information in the form of radio-frequency study at LBNL. The electrocatalysts are added to a waves and optical images. Our project goal is to state-of-the-art air electrode and performance is- develop an inexpensive single-chip frequency agile RF evaluated in the three-electrode configuration in the transceiver operating at the 2.4 GHz range - a absence of zinc. Two candidates appear promising and universally accepted unlicensed band - with data rates will be incorporated into full zinc-air cells for testing. up to 250 Kbps and an approximate range of 50 feet. We have previously demonstrated successful circuit Keywords: Zn/Air Batteries, Electrochemistry, blocks and will be seeking to use a higher performance Electrocatalysts, Electrodes CMOS 0.35 micron process to achieve lower power consumption and higher integration density. For the optoelectronic imaging portion of this project, we will investigate the 'active pixel" architecture. This architecture uses photodiode sensors which can be made in a native CMOS process. The imaging array requirements (pixel size and count, spectral responsivity, speed, signal-to-noise ratio, dynamic

109 Office of Energy Research

240. MICROMAGNETIC STRUCTURES (LBL95-12) and petroleum imports while creating a new growth $378,000 industry. DOE Contact: Walter M. Polansky, (301) 903-5995 Keywords: Zn/Ni Batteries, Electric Vehicles, Alkaline LBNL Contact: Neville Smith, Accelerator and Electrolytes, Zn and Ni Electrodes Fusion, (510) 486-5423 242. CATALYTIC CONVERSION OF CHLORO- This goal of this project is to produce a powerful and FLUOROCARBONS OVER PALLADIUM- unique tool for microscopic imaging of magnetic CARBON CATALYSTS (LBL95-45) materials (a tool which will take full advantage of the $275,000 capabilities of the ALS), and to use this tool to develop DOE Contact: Walter M. Polansky, new magnetic materials for high density information (301) 903-5995 storage. The microscope is based on a full field LBNL Contact: Gabor Somorjai, Materials photoelectron emission technique, and magnetic Sciences, (510) 486-4831 information is extracted using a synchrotron radiation spectroscopy known as X-ray Magnetic Circular Chlorofluorocarbons must be substituted as refrigerants Dichroism. The microscope will have elemental and and chemicals because of their adverse health effects chemical selectivity, combined with surface sensitivity, (ozone depletion and other effects). The hydrodechlori- and the ability to measure surface magnetic moments. nation (HDCI) of C2F4C, is a technology that uses This combination of features is unique in the array of palladium catalyst supported on carbon. This research tools currently used to study magnetic materials. The investigates the structure and bonding of reactants and project uses LBNL's expertise in design and operation of products on palladium crystal surfaces that are also synchrotron instrumentation, beamlines, and experi- used as model catalysts. The elementary steps of the mental end stations in the production of artificially reaction and its mechanism are explored this way. The engineered magnetic microstructures. causes of catalyst deactivation is being studied, along with the use of promoters to inhibit it. The roles of the Keywords: Micromagnetics, Information Storage, carbon support and the palladium-carbon interface are Magnetic Imaging, Photoelectron also of interest as they influence the catalytic reaction Emissions rate and selectivity.

241. DEVELOPMENT OF ZINC/NICKEL OXIDE Keywords: Chlorofluorocarbons, Pd Catalysts, BATTERIES FOR ELECTRIC VEHICLE Hydrodechlorination, Reaction Mechanisms APPLICATIONS (LBL95-27) $42,000 243. IONICALLY CONDUCTIVE MEMBRANES FOR DOE Contact: Walter M. Polansky, OXYGEN SEPARATION (LBL97-03) (301) 903-5995 $125,000 LBNL Contact: Frank McLarnon, Energy DOE Contact: Walter M. Polansky, Conversion and Storage, (510) 486-4636 (301) 903-5995 LBNL Contact: Steven J. Visco, Materials The goal of this project is to develop a light-weight, Sciences Division, (510) 486-5821 rechargeable battery for electric vehicles. This battery uses an alkaline electrolyte, a zinc negative electrode The global market for industrial oxygen is estimated at and a nickel oxide positive electrode. It has two major $20 billion annually. The dominant technology for the advantages over competing types such as cadmium/ production of commercial oxygen is cryogenic distilla- nickel oxide (nickel-cadmium) and metal-hydride/nickel tion. The high capital equipment costs for cryogenic 02 oxide (nickel-metal hydride): it delivers more energy per separation limits this technology to large installations. unit battery mass and costs less to produce. LBNL has Accordingly, industrial suppliers of oxygen are highly developed a novel electrolyte for the zinc/nickel oxide motivated to develop technologies that can satisfy battery that extends its useful life to several hundred increasing demand for oxygen through smaller scale charge-discharge cycles. Additional improvements to plants. One approach under development elsewhere is lower the battery mass and to increase the ability of the the use of mixed ionic-electronic ceramics; when such electrolyte to wet the electrodes are being investigated. ceramic electrolytes are exposed to compressed air on If these efforts are successful, full-size electric vehicle one side and ambient pressure on the other, oxygen batteries will be built for testing. A superior zinc/nickel diffuses through the mixed conductor from the oxide battery could be the key to inexpensive and compressed side to the low pressure side due to the durable electric vehicles which will reduce air pollution chemical potential gradient of oxygen across the membrane. The drawback to this technology is the need

110 Office of Energy Research

for a compressor which raises issues of noise and from being made. Recently, breakthroughs in the reliability. Another problem is that permeation delivers heteroepitaxial growth of gallium nitride (GaN) and its ambient pressure oxygen. In contrast, we propose the alloys with indium and aluminum have changed the blue efficient electrolytic extraction of oxygen from air using and green LED technology outlook. Formerly, it was novel thin-film structures consisting of high strength believed that Ill-V nitride layers had too high a defect ionic membranes supported on porous, catalytic density to function as LEDs. Nevertheless, a Japanese electrodes. Using this technology, high purity 02 can be company (Nichia) has developed a family of blue and electrochemically pressurized as an integral part of the green LEDs based on GaN that are bright and efficient. separation process. The simplicity of operation of an For the last two years, Japanese companies have been electrolytic 02 generator promises high reliability as well manufacturing and selling blue GaN LEDs in bulk as low cost. Still, to survive as a commercial process, quantities. This project is a collaboration with Hewlett- this approach must be cost-competitive to cryogenic Packard Company (HP), the leading producer of LEDs, production of 02. Key to success is highly efficient to investigate the fundamental light-emitting operation (low power consumption) of the device along mechanism. Epitaxial thin film growth, including with low fabrication costs. Power losses in the specialized structures and doping series and basic electrolytic oxygen cell will be related to ohmic losses parametric characterization, will be performed in the across the electrolyte membrane, charge transfer industrial research laboratories of HP Highly polarization at the electrode/electrolyte interfaces, and homogenous, reliably reproducible, and stable metal mass transfer polarization across the electrodes. The organic vapor phase epitaxial growth processes have LBNL approach addresses the above issues in such a been established at HP laboratories. Highly specific way that both scientific and technical success are likely. spectroscopic characterization and analysis aimed at The LBNL team has initiated preparation of porous revealing the basic principles underlying doping and substrates suitable for colloidal deposition. High recombination will be performed by LBNL's Materials temperature furnaces are being installed for sintering of Sciences Division, supporting key DOE missions in bilayer structures suitable for high oxygen flux in an materials research. electrolytic oxygen generator. The LBNL investigator recently met with the principal investigator for the Keywords: LEDs, Semiconducting Materials, Gallium industrial partner to discuss the timeline for the Nitride, Light Emitting Mechanisms, development plan. A tentative date of October 1997 has Heteroepitaxial Growth, Blue Emitting be agreed upon for the LBNL team to travel to industrial Diodes, Red Emitting Diodes, Green partner's laboratory in order to discuss the development Emitting Diodes plan in detail, and to ensure maximum productivity of the collaborative effort. This research supports the DOE 245. COMBINATORIAL DISCOVERY AND mission in materials research and applications. OPTIMIZATION OF NOVEL MATERIALS FOR ADVANCED ELECTRO-OPTICAL DEVICES Keywords: Oxygen, Membranes, Separation, Ceramic (LBL97-18) Electrolytes, Catalytic Electrodes, Oxygen $125,000 Generators DOE Contact: Walter M. Polansky, (301)903-5995 244. LIGHT EMISSION PROCESSES AND DOPANTS LBNL Contact: Xiao-Dong Xiang, Materials IN SOLID STATE LIGHT SOURCES (LBL97-13) Sciences Division, (510) 486-4864 $125,000 DOE Contact: Walter M. Polansky, Advanced materials are the building blocks of the (301) 903-5995 emerging photonic technologies which are the LBNL Contact: Eugene E. Haller, Materials foundation for a new industrial base. Complex oxide Sciences Division, (510) 486-5294 ceramics (ternaries and higher order compounds) exhibit a wide range of technologically significant Light emitting diodes (LEDs) functioning in the red and properties such as the electro-optic effect. The rapid infrared have been manufactured in large quantities expansion in the types of phenomena exhibited by since the 1960s. However, until very recently, only very modern advanced ceramics has revived interest in the inefficient and dim LEDs were available in the green use of complex oxides for advanced optical device and, especially, in the blue. Although there are a applications. This project directly supports DOE's handful of semiconducting materials with sufficiently interests in materials research for advanced ceramic wide bandgaps to function in principle in the blue region applications. However, due to the complexity of multi- of the spectrum, fundamental material properties and component oxides, searching for new materials or limitations have prevented bright and efficient diodes optimization of existing materials has become a

111 Office of Energy Research

forbidding task for the materials community. This manufacturing of the next generation of microelectronic project will: (1) use the method of combinatorial integrated circuits (ICs). These include: (1) gettering of synthesis and screening, recently developed at LBNL, to impurities, where the goal is to identify and evaluate evaluate a wide range of oxide materials and implantation-based schemes for generating stable compounds and optimize the advanced oxide materials gettering sites for deleterious impurities within silicon for electro-optical devices; and (2) use heteroepitaxial wafers; (2) dielectrics, where the aim is to develop and thin film growth methods, developed at NZAT, to test thin dielectric films for compatibility with shallow fabricate advanced oxide electro-optical devices based junction formation; and (3) metallization, where the on search and optimization results. The goal of this challenge is to eliminate stress-induced metal failures. project is to produce commercially viable advanced In this research, the feasibility of using ion- electro-optical devices. If successful, this project will implantation-based approaches for solving these play an important role in forming a strong foundation for problems during manufacturing will be evaluated. the emerging large scale integrated optics device industry. Keywords: Ion Implantation, Integrated Circuits, Semiconductor Manufacturing Keywords: Photonic Technologies, Oxide Ceramics, Mutli-Component Oxides, Electro-Optical 248. RAPID PROTOTYPING OF CERAMICS Devices, Synthesis, Thin Films (ORL94-95) $153,000 246. DEVELOPMENT OF A THIN-FILM BATTERY DOE Contact: Walter M. Polansky, POWERED HAZARD CARD AND OTHER (301) 903-5995 MICROELECTRONIC DEVICES (ORL94-39) ORNL Contact: Robert Lauf, Engineering $74,000 Technology Division, (423) 241-2102 DOE Contact: Walter M. Polansky, (301) 903-5995 The goal of this project is to develop fundamental ORNL Contact: John Bates, Solid State, knowledge and apply that knowledge to the technology (423) 574-6280 of rapid product realization for structural ceramic components. A major part of the effort is directed to The goals of this research project are to investigate the modifying solid freeform fabrication techniques to feasibility of powering integrated circuit chips and produce sinterable ceramic green bodies rather than compact microelectronic-based devices with thin-film, plastic models. The program also recognizes the crucial rechargeable batteries that can withstand temperatures role of advanced computational techniques for creating of up to 200°C, and to determine and eliminate and manipulating the large data files needed to obstacles to their manufacturability. Since they have adequately represent complex three-dimensional high energies per unit of volume and mass and because components with the necessary resolution. they are rechargeable, thin film lithium batteries have potentially many applications as small power supplies in Keywords: Freeform Fabrication, Rapid consumer and medical microelectronic products. This Manufacturing, Ceramics research into battery technology will enable the reduction in size and improvement in performance of 249. DEVELOPMENT OF A THIN FILM BATTERY existing microelectronic devices. POWERED TRANSDERMAL MEDICAL DEVICE (ORL95-11) Keywords: Thin-Film Batteries, Microelectronics, $187,000 Electronic Devices DOE Contact: Walter M. Polansky, (301) 903-5995 247. ION IMPLANTATION PROCESSING ORNL Contact: John B. Bates, Solid State TECHNOLOGIES (ORL94-72) Division, (423) 574-6280 $136,000 DOE Contact: Walter M. Polansky, Heart and brain activity are monitored by measuring (301) 903-5995 microvolt signals developed on the surface of the skin ORNL Contact: Tony Haynes, Solid State, using transdermal electrodes. The first objective of this (423) 574-2858 project was to develop a thin-film battery powered preamplifier that would attach directly to these The objective of this project is to cooperate in ion electrodes so that the small electrocardiogram (EKG) implantation research and related processing of and electroencephalogram (ECG) signals could be semiconductors to accelerate the development cycle for amplified before transmission to the recording unit. three critical technologies required for the These "active" electrodes will eliminate the effect of

112 Office of Energy Research interference from ac pickup in the long cables from the 251. DEVELOPMENT OF HIGH-TEMPERATURE recording unit and improve the reliability in diagnosing SUPERCONDUCTING WIRE USING RABITS heart or brain malfunctions. By incorporating batteries COATED CONDUCTOR TECHNOLOGIES into the circuit to power the amplifiers, no change to (ORL97-02) existing EKG or ECG recording equipment is required. $100,000 A thin-film lithium battery was developed that exceeds DOE Contact: Walter M. Polansky, the requirements of Teledyne's transdermal-electrode (301) 903-5995 application. The battery, which is based on a LiCoO2 ORNL Contact: David K. Christen, Solid State cathode, was fabricated directly onto the backside of the Division Donald M. Kroeger, Metals and multi-chip modules developed by Teledyne as a Ceramics Division, (423) 574-6269 prototype electrode preamplifier. This was the first demonstration of integration of thin-film batteries into This project is developing a recent breakthrough at Oak electronic devices. When developed, the active Ridge National Laboratory that offers a potential new electrodes will significantly improve the reliability of route to the fabrication of high-temperature EKG and ECG diagnostic measurements and thereby superconducting (HTS) wires for power applications. help to improve the quality of patient care at a lower The new process produces high-Tc coatings that have cost. The second objective of this project is to high critical-current densities at liquid nitrogen demonstrate manufacturing of thin-film batteries in a temperatures, and enable operation in substantial pilot scale facility at Teledyne. The cathode and magnetic fields. The present approach exploits the electrolyte films deposited at Teledyne are being growth of crystalline biaxially-aligned coatings on shipped to ORNL for a comparison of their properties oriented metal tapes produced by simple thermo- with those grown at ORNL. To date, Teledyne has mechanical processing. The tapes start with fabricated excellent LiCoO2 cathode films over areas inexpensive polycrystalline metals or alloys that are nearly 40 times larger than possible at ORNL. Batteries biaxially aligned by deformation rolling and thermal fabricated at Teledyne will be evaluated at ORNL. If annealing treatment, followed by the epitaxial deposition they meet the rigid requirements of the medical device, of thin, passivating buffer layers. The project team is full-scale manufacturing will follow. Teledyne has investigating the scientific and technical feasibility of licensed ORNL's thin-film battery technology for making long-length coated conductors that can provide application in medical devices. The work performed in operating characteristics that are currently unattainable this project supports DOE's Basic Energy Sciences by any electrical conductor, including present prototype programs in advanced battery technology and advanced HTS tapes that utilize the "powder-in-silver-tube" ceramics. fabrication approach. The research focuses on both the simplification and optimization of oxide buffer layers on Keywords: Thin-Film Batteries, Transdermal Medical reactive metals, and specifically will evaluate Devices, Lithium, Multi-Chip Modules (co)evaporation techniques for both the buffer layer(s) and the superconductor coatings. 3M has an 250. RAPID PROTOTYPING OF BIOCERAMICS FOR established experience base in high-rate deposition of IMPLANTS (ORL95-12) other materials using this manufacturing technology. $64,000 Southwire is the leading U.S. manufacturer of utility wire DOE Contact: Walter M. Polansky, and cable, and is a retailer of underground transmission (301) 903-5995 cables (a prime first candidate for HTS insertion). A ORNL Contact: Ogbemi Omatete, Metals and cost-effective route to high-temperature Ceramics Division, (423) 576-7199 superconducting wires would provide substantial national energy benefits in the technology of electric The goal of this research is to combine the ORNL power production, storage, and distribution. gelcasting process and an injection stereolithography Superconducting transmission lines alone would enable process to make a rapid manufacturing system suitable 2-3 times the power transfer into urban areas without for the fabrication of limited-production ceramic the need for additional rights-of-way and without components for implants and prostheses. This project significant losses to resistance. Other applications, such will complement a related effort led by Argonne National as power transformers, motors, current limiters, and Laboratory in the conversion of CAT/MRI data sets into magnetic energy storage, are projected to produce a format suitable for rapid freeform fabrication markets of tens of billions of dollars per year. This processes. project will help DOE's Office of Utility Technologies,

Keywords: Ceramics, Gelcasting Process, Rapid Manufacturing, Freeform Fabrication

113 Office of Energy Research

Energy Efficiency and Renewable Energy program to 254. NOVEL METHODS FOR FABRICATION COST develop high-temperature superconductors. REDUCTION OF PRESSURE INFILTRATION CAST METAL MATRIX COMPOSITE Keywords: Superconducting Wires, Coatings, COMPONENTS (ORL95-1) Metalworking, Coated Conductors, $192,000 Electrical Equipment, Distribution and DOE Contact: Walter M. Polansky, Transmission, High Temperature (301) 903-5995 ORNL Contact: James Hansen, Engineering INSTRUMENTATION AND FACILITIES Technology Division, (423) 241-2102

252. MICRO-SPECTROSCOPY FACILITY FOR NEW The goal of this project is to develop pressure infiltration INFRARED IMAGING MATERIALS (BNL94-60) casting as a method to manufacture high quality metal $91,000 matrix composite castings at high production rates. The DOE Contact: Walter M. Polansky, manufacturing demonstration component of the project (301) 903-5995 is a lightweight (60 percent reduction or 20 pound BNL Contact: Gwyn Williams, NSLS weight savings versus cast iron calipers), high modulus, (516) 344-7529 particulate reinforced aluminum brake caliper.

Brookhaven National Laboratory is developing a custom Keywords: Pressure Infiltration Casting, Manufacture, synchrotron beamline facility for characterizing infrared Metal Matrix Composites sensor technology materials. New materials for high performance and/or low cost infrared imaging systems 255. ULTRA-PRECISION AUTOMATED will be developed and tested. The testing involves MEASUREMENT FOR MANUFACTURING infrared microspectroscopy using infrared synchrotron (ORL95-08) radiation as the source for the microscope. Synchrotron $75,000 radiation is 1000 times brighter than conventional DOE Contact: Walter M. Polansky, thermal infrared sources, making this a unique facility. (301) 903-5995 ORNL Contact: C. Thomas, Fusion Energy Keywords: Micro-spectroscopy, Infrared, Imaging Division, (423) 574-1155 Materials, Synchrotron Beamline Project goal is to demonstrate a new level of automated 253. DEVELOPMENT OF ENVIRONMENTALLY process control, noncontact measurement technology CONSCIOUS MACHINING FLUIDS for the United States manufacturing sector. The (ORL94-91) immediate goal is proof of concept for intelligent $204,000 automated electronic interferometry inspection of digital DOE Contact: Walter M. Polansky, microchips with a resolution better than the lithographic (301) 903-5995 mask resolution (e.g., a transverse resolution of ORNL Contact: Thomas Morris, Metals and 200 nanometers and a longitudinal resolution of Ceramics, (423) 241-2796 20 nanometers). This will allow automated 3-dimensional inspection of the chips between The objective of this project is to develop required processing steps to insure success of the processing at cutting fluids for ceramic and other advanced materials each step; immediately identify process failures; save that are more environmentally benign and will reduce or time, money, and energy; improve quality and yield by eliminate the environmental problems associated with eliminating defective chips early in the processing; and management and disposal of these cutting fluids. The immediately identify process failures. The intention is to specific goal of the project is to develop a method to provide a totally automated, rapid, on-line inspection degrade synthetic cutting fluids and reduce their total capability to automatically detect and sort defective organic carbon (TOC) content and chemical oxygen chips or call for human intervention. This technology demand (COD) to allow for final disposal in municipal can be extended to inspection and process control for sewage treatment facilities. Water-based industrial all kinds of precision components, particularly for the fluids can have excessively high TOC (ca. automotive, electronics, and defense industries. Some >15,000 PPM), thus making their treatment especially examples of additional uses include: automated challenging. inspection of precision machined parts; automated inspection of heads and platters for hard disk drives Keywords: Cutting Fluids, Ceramics, Machining, (where some tolerances are starting to approach the Environmental sub-micron level); and automated noncontact inspection

114 Office of Energy Research of aircraft wing sections and automotive body panels on of filtration elements and solid phase extraction a more macroscopic level, elements that can be monolithically integrated onto electrophoresis and chromatographic structures Keywords: Ultra-Precision Measurements, Automated pioneered at ORNL. Successful demonstration of these Process Control, Manufacturing, Inspection additional functional elements on integrated microfabricated devices will allow lab-on-a-chip technologies 256. NEURAL NETWORK MODEL (ORL95-90) to address real world samples that would be $248,000 encountered in process-control environments. The DOE Contact: Walter M. Polansky, resultant technology will have broad application to (301) 903-5995 industrial environmental monitoring problems such as ORNL Contact: Gerald Ludtka, (423) 574-5098 monitoring municipal water supplies, waste-water effluent from industrial facilities, or monitoring of run-off The goal of this project is to significantly reduce the from agricultural activities. The technology will also be required number of iterations in the sheet metal forming adaptable to manufacturing process control scenarios. die design process, a process typically involving This project supports DOE missions in environmental extensive and costly physical prototyping. The project quality and energy efficiency. employs a collection of emerging computational technologies such as digital simulations of deformation Keywords: Microfabricated Instrumentation, Chemical processes, neural networks, high-performance Sensing, Industrial Process Control, 'Lab- computing, and 3-dimensional optical metrology in on-a-Chip Devices," Chemical Analysis, order to achieve accurate and timely computations Environmental Monitoring, Manufacturing during the design process as well as during the control Processes of the stamping process so as to eliminate a large fraction of the presently required design iterations. 258. MODELING AND SIMULATION OF ADVANCED SHEET METAL FORMING (PNL94-38) Keywords: Neural Networks, Die Design, Sheet Metal $170,000 Forming, Optical Metrology, Stamping DOE Contact: Walter M. Polansky, Process (301) 903-5995 PNNL Contact: Mark Smith, Materials & 257. MICROFABRICATED INSTRUMENTATION FOR Chemical Sciences, (509) 376-2847 CHEMICAL SENSING IN INDUSTRIAL PROCESS CONTROL (ORL97-08) This project will enhance numerical modeling and $99,000 simulation of advanced sheet metal forming processes, DOE Contact: Walter M. Polansky, allowing rapid elevated temperature processing of (301) 903-5995 lightweight aluminum alloy sheet. In this project, ORNL Contact: J. Michael Ramsey, Chemical improved material deformation models and predictive and Analytical Sciences Division, codes for advanced forming processes will be (423) 574-5662 developed. Development of the new capabilities will allow the manufacturing industries to optimize the The monitoring of chemical constituents in manufac- component and tooling designs and improve the turing processes is of economic importance to most forming processes without costly trial and error industries. The monitoring and control of chemical development of the advanced forming technology. constituents may also be of importance for product Implementation of this modeling and forming quality control or, in the case of process effluents, of technology will enhance the competitiveness of U.S. environmental concern. The most common approach industry. now employed for chemical process control is to collect samples which are returned to a conventional chemical Keywords: Advanced Sheet Metal Forming, Modeling analysis laboratory. The objective of this project is to and Simulation, Lightweight Al Alloy demonstrate the use of microfabricated structures, Sheets, Manufacturing, Competitiveness of referred to as 'lab-on-a-chip' devices, that accomplish U.S. Industry chemical measurement tasks that emulate those performed in the conventional laboratory. The devices envisioned could be used as hand portable chemical- analysis instruments where samples are analyzed in the field or as emplaced sensors for continuous "real-time" monitoring. This project will focus on the development

115 Office of Energy Research

MATERIALS PROPERTIES, BEHAVIOR, 260. PREVENTION/ELIMINATION OF METAL- CHARACTERIZATION OR TESTING WATER EXPLOSIONS IN ALUMINUM CASTING PITS (ORL92-05) 259. NEXT GENERATION CORROSION INHIBITORS $174,000 FOR STEEL IN CONCRETE (BNL95-12) DOE Contact: Walter M. Polansky, $50,000 (301) 903-5995 DOE Contact: Walter M. Polansky, ORNL Contact: Rusi P. Taleyarkhan, (301) 903-5995 Engineering Technology Division, BNL Contact: Hugh Isaacs, Applied Science (423) 576-4735 (516) 344-4516 Metal-water or steam explosions in aluminum industry Steel-reinforced concrete is the most widely used casting pits have caused numerous injuries and construction material in the world. This is almost an fatalities, and significant damage and destruction of ideal composite, with the steel providing tensile strength infrastructure over the past fifty years. Traditionally, and the alkaline concrete imparting passivity to the industry has attempted to prevent explosions by using steel. However, passivity can be compromised by the an empirical-based approach involving the coating of ingress of chlorides from a marine environment or from sensitive surfaces with materials like Tarset Standard de-icing salts. To address this problem, corrosion (TS). However, due to environmental concerns and inhibitors are added to the concrete mixture, usually as other reasons, TS is being discontinued from simple inorganic anions (e.g. nitrite). Both the production, leaving industry with the task of evaluating mechanism of corrosion in a concrete environment and and finding alternate materials. As part of this project the action of inhibition are not well understood. The goal with the Aluminum Association (AA), ORNL is of this project is to elucidate the action of corrosion and investigating how steam explosions initiate over specific the behavior of inhibitors. The objective of the study will surfaces, and what other coatings and novel methods ultimately be to develop more effective inhibition, may be appropriate as alternatives to TS. Work possibly by the use of mixed anodic/cathodic inhibitors completed has resulted in the development and or altering the form in which the inhibitors are added. validation of a unique apparatus that, at significant cost Corrosion measurements are being made of the anodic reduction, accurately and rapidly simulates in a and cathodic kinetics taking place in concrete, which laboratory environment the interaction of molten describe the processes occurring with and without aluminum contacting various submerged surfaces inhibitors. Nitrite inhibitors have been found to display without attendant safety problems associated with field different degrees of effectiveness at various stages experiments involving molten aluminum pours in water- during the development of corrosion. In sufficient filled containers. While further testing and theoretical quantities, the inhibitors maintain passivity. However, model development still need to be done, they apparently have little action on the very early unprecedented insights have been obtained on key stages of passivity breakdown. At a later stage, when phenomenological issues. This has enabled the corrosion is well developed, corrosion is again development of a novel approach for conclusive influenced by nitrite additions. Very small quantities explosion prevention. A patent has been filed and distinctly reduce the corrosion rates, whereas large granted for this novel, environmentally-friendly, cost- additions again act to produce passivity and no effective approach based on knowledge of fundamentals corrosion. Efforts are now underway to define more of the physics of explosion initiation. Field closely the critical factors determining the differences in demonstrations are planned. This project supports behavior. X-ray absorption near edge measurements DOE's energy-related mission to develop a more will also be performed to examine the effect (if any) of energy-efficient metal-casting operation. Additionally, inhibitors on the structure and chemistry of the passive this work is expected to provide a better physical oxide. Research in this area supports the DOE mission understanding of entrapment-boiling heat transfer that in materials characterization and processing. could be applied to safety improvements in DOE and commercial nuclear reactors. Keywords: Steel-Reinforced Concrete, Corrosion, Corrosion Inhibitors, Passivation Keywords: Aluminum Production, Aluminum Casting Explosion, Molten Aluminum, Heat Transfer, Injuries and Fatalities

116 Office of Energy Research

261. IN-LINE ALUMINUM SENSORS (ORL95-04) in the alloys; (2) examining the oxidation performance of $113,000 these newly-developed alloys; and, (3) relating the DOE Contact: Walter M. Polansky, microstructural observations to the observed (301) 903-5995 performance. ORNL Contact: Jack Young, Chemical & Analytical Sciences, (423) 574-5241 Keywords: Turbines, Ni-Based Superalloys, Oxidation, Yttrium Alloying, Microstructure The objective of this project is to develop in-line sensors for commercial aluminum electrolysis cell operation. 263. ATOMIC SCALE STRUCTURE OF ULTRATHIN The sensors to be developed will be of a Raman MAGNETIC MULTILAYERS AND spectral type. The research goal is to develop CORRELATION WITH RESISTANCE, GIANT technology which will allow measurement of soluble MAGNETORESISTANCE, AND SPIN- alumina, bath ratio and bath temperature. These in-line DEPENDENT TUNNELING (ORL97-03) measurements will be inputs to new process control $100,000 algorithms that can then be developed to improve the DOE Contact: Walter M. Polansky, efficiency of aluminum electrolysis operations thereby (301) 903-5995 reducing energy consumption. Such energy saving is in ORNL Contact: William H. Butler, Metals and line with the goals of DOE. The improved control Ceramics Division, (423) 574-4845 algorithm will also lead to a reduction in the anode effect which results in wasted energy and fluorocarbon Giant Magnetoresistance (GMR) and Spin-Dependent emission. Reduction of potentially hazardous Tunneling (SDT) are two recently discovered environmental gases is also a goal of DOE. Along with phenomena that are providing important new insights the development of these sensors, the basic chemistry into how spin affects the transport of electrons in of the melts will be studied to gain knowledge of materials. These phenomena have the potential to spark speciation and effect of impurities on the process revolutionary advances in several important efficiency. A critical parallel study will be carried out to technologies and both require the controlled deposition develop sheath materials that will have a useful lifetime of ultrathin films. In order to realize the scientific and (6 months) in cryolite melts. With such sheath technological potential of these phenomena, it is materials, the long-term measurement of temperature necessary to relate the spin-dependent transport by standard techniques can also be accomplished. properties to the spin-dependent electronic structure of the deposited structures. Since spin dependent Keywords: Aluminum Electrolysis Cell, In-Line transport is very sensitive to structure at that scale, an Sensors, Manufacture understanding of the deposited structures at the atomic scale is required to accomplish that goal. Recent 262. THE ROLE OF YTTRIUM IN IMPROVING THE advances in electronic structure theory allow the OXIDATION RESISTANCE IN ADVANCED calculation of spin-dependent transport. The missing SINGLE CRYSTAL NICKEL-BASED key, however, is atomic-scale characterization of the SUPERALLOYS FOR TURBINE APPLICATIONS deposited films. Through a close collaboration between (ORL95-07) theory and experiment, the objective of this project is to $149,000 determine the physical, chemical, and magnetic DOE Contact: Walter M. Polansky, structure of GMR and SDT films and to relate their (301) 903-5995 structure to their magnetic and transport properties. ORNL Contact: Kathleen Alexander, Metals This will be achieved by combining a uniquely powerful and Ceramics Division, (423) 574-0631 set of characterization tools, (X-ray Reflection and Diffraction, Atom- Probe Microscopy, Z-Contrast The focus of this project is to examine the role of yttrium Electron Microscopy with Electron Energy Loss and other alloying elements on the microstructure and Spectroscopy, and Electron Holography) with first- oxidation performance of improved single crystal nickel- principles computer codes that are capable of based superalloys for advanced turbine applications. calculating the spin-dependent conductivity for realistic Anticipated improvements from these new alloys systems. The industrial partners (Honeywell Solid State include enhanced durability and performance at the high Electronics Center and Nonvolatile Electronics Inc.) are temperatures required to improve energy efficiency. uniquely qualified to optimize their deposition processes Specific technical goals include: (1) identifying the and to relate the structures they deposit to the observed partitioning behavior of the elemental additions in these spin-dependent transport. Success in this project should superalloys before and after burner rig and engine tests lead to better read sensors for magnetic disk drives, a and the effect on the misfit energy between the phases new type of non-volatile radiation resistant magnetic

117 Office of Energy Research

random access memory device, and better position and growing market currently estimated to be between $1.2 motion sensors for numerous industrial, transportation, to $1.5 billion annually. and consumer product applications. Additionally, this work enhances DOE's basic materials sciences Keywords: Biologically Suitable Metallic Devices, programs in magnetic structures and advanced Tissue Regeneration, Health-Related characterization methods. Technology Devices

Keywords: Giant Magnetoresistance, Spin-Dependent ADVANCED ENERGY PROJECTS PROGRAM Tunneling Electron Transport, Magnetic Multilayers, Atomic Scale Structures, The Division of Advanced Energy Projects (AEP) Applications provides support to explore the feasibility of novel, energy-related concepts that evolve from advances in 264. PROCESSING/PROPERTY RELATIONSHIPS IN basic research. These concepts are typically at an early CENTRIFUGALLY CAST AL-METAL MATRIX stage of scientific development and, therefore, are COMPOSITES (MMC) (PNL94-02) premature for consideration by applied research or $245,000 technology development programs. The AEP also DOE Contact: Walter M. Polansky, supports high-risk, exploratory concepts that do not (301) 903-5995. readily fit into a program area but could lead to PNNL Contact: Ed Courtright, Material applications that may span several disciplines or Sciences, (509) 375-6926 technical areas.

The goal of this project is to develop cost-effective The Division provides a mechanism for exploring the selectively reinforced metal matrix processing conversion of basic research results into applications technology. Light alloy metal matrix composites that could impact the Nation's energy economy. AEP reinforced with silicon carbide or alumina particulates does not support ongoing, evolutionary research or can replace steel in many automobile applications, and large scale demonstration projects. Technical topics the corresponding reduction in vehicle weight translates include physical, chemical, materials, engineering, and to a proportional increase in gas mileage. This project biotechnologies. Projects can involve interdisciplinary concentrates on understanding the microstructure of approaches to solve energy-related problems. The DOE centrifugally cast MMC's because the process offers the Contact for this program is Walter M. Polansky, unique capability to distribute the particle phase in 301/903-5995. regions or zones where the reinforcements will have the greatest benefit. Emphasis will be placed on DEVICE OR COMPONENT FABRICATION, understanding processing/property relationships and in BEHAVIOR OR TESTING determining how these can be controlled to optimize selectively reinforced composite structures. 266. COMPOSITE MAGNETOSTRICTIVE MATERIALS FOR ADVANCED AUTOMOTIVE Keywords: Metal Matrix Processing, Centrifugal MAGNETOMECHANICAL SENSORS Casting, Al-Metal Composites $449,000 DOE Contact: Walter M. Polansky, 301/903-5995 265. BIOACTIVE AND POROUS METAL COATINGS Ames Laboratory Contact: David C. Jiles, FOR IMPROVED TISSUE REGENERATION 515/294-9685 (PNL95-23) $191,000 There is a well established need for torque sensors for a DOE Contact: Walter M. Polansky, variety of applications in automobiles. Such sensors (301) 903-5995 can be used for electronic control of the vehicle by PNNL Contact: Allison Campbell, Materials & monitoring steering and drive train torques. In this Chemical Sciences, (509) 375-2180 project, new highly magnetostrictive materials are being investigated for use in advanced steering systems. Such The goal of this project is to combine complementary sensors will eliminate the need for maintaining a technologies and conduct a testing program which pressurized hydraulic power steering system and will would provide information necessary to develop novel improve fuel efficiency by 5%. These sensors will need health-related technology devices. If the laboratory to meet stringent specifications such as the ability to research demonstrates that metals or alloys can be operate over a range of temperatures between minus reproducibly and uniformly coated using PNNL's unique 40°C and plus 85°C, be able to survive unexpected technology and the biologically suitable metallic or alloy mechanical shocks of up to 500 N and operate under devices coated with the technology are shown to have continual vibrational forces of 150 N. In addition, the improved performance in selected animal studies and sensors must be able to sustain overload torques of 135 clinical trials, then the potential products will target a N.m without malfunctioning or significantly changing

118 Office of Energy Research sensitivity over the normal operating range of +/- 10 frequencies will be constructed and evaluated with the N.m. Analysis of the relationship between the cooperation of an industrial affiliate. magnetomechanical effect (the change in magnetization with stress) and the magnetostriction (particularly the Keywords: Solar Cells, Photovoltaic, MOMBE, rate of change of strain with magnetic field) has shown Metalorganic Molecular Beam Epitaxy that highly magnetostrictive materials with low anisotropy, and hence high permeability, form the most 268. INVESTIGATION OF HIGH EFFICIENCY MULTI promising class of materials from which to develop such BAND GAP MULTIPLE QUANTUM WELL high performance sensors. This project is therefore SOLAR CELLS investigating the fabrication of composite materials $225,000 consisting of the highly magnetostrictive material DOE Contact: Walter M. Polansky, 301/903-5995 Terfenol-D in a high-strength matrix material, in order to City College of City University of New York meet the performance specifications for these torque Contact: Robert Alfano, 212/650-5532 sensors. This project will investigate and develop multiple Keywords: Magnetostrictive Materials, Torque quantum well (MQW) solar cells which are expected to Sensors, Terfenol-D reach much higher efficiency than that obtained from conventional bulk solar cells by reducing radiative and 267. ENERGY RELATED APPLICATIONS OF nonradiative relaxation processes through resonant SELECTIVE LINE EMITTERS tunneling. The maximum energy conversion efficiency $266,000 of a conventional bulk solar cell is limited to less than DOE Contact: Walter M. Polansky, 301/903-5995 -33% because of its single band gap. Using a novel Auburn University Contact: M. Frank Rose, MQW-based solar cell with multi band gaps, one 334/844-5894 expects to enhance the maximum energy efficiency to -72%. These high efficiency MQW solar cells have the Infrared heat sources are used extensively for many potential of being widely used in compact computers, processes in industry. From initial work, it appears space power supplies, micro-scale motors, consumer feasible to develop intense infrared sources based upon products, home electronic devices, guide signs, and electronic transitions in compounds of the rare earths, other renewable energy applications. In preliminary which tend to radiate efficiently at discrete wavelengths studies, we have measured carrier dynamics and band rather than a continuum. This project is aimed at gap structures for GaAs, InP and their alloys, and conducting the basic and exploratory research that will calculated the resonant tunneling time and the barrier allow the development of high intensity, discrete potential design criteria for achieving maximum energy frequency infrared sources that are custom tailored to conversion efficiency in MQW structures. Based on specific industrial processes. This will be accomplished these measurements and calculations, we have by investigating and characterizing the emissive designed several GaAs- and InP-based MQW solar cell properties of the rare earths in inert forms such as structures which have been fabricated using the MBE oxides, borides, carbides, or nitrides. The Center for the facility at CCNY. The current-voltage (I-V) Rare Earth Elements at the DOE Ames Research characteristics of the fabricated GaAs/AIGaAs MQW Laboratory will be used as the source of information for solar cells have been measured, and an enhancement selection of suitable rare earth elements and of energy efficiency for the MQW solar cells over that of compounds. Fibrous inert compounds of the rare earths the conventional bulk solar cells has been observed. will be formed as necessary. Oxide fibers can be formed This project will enhance these studies and develop high by soaking activated carbon fibers in a suitable liquid efficiency multiband gap MQW solar cells. We will compound of the rare earth, such as a nitrate of the investigate resonant tunneling times for GaAs/AIGaAs material. Since activated carbon fibers can be greater and InGaAs/lnP MQW structures to make sure that the than 70% porous, a substantial fraction of the liquid can resonant tunneling process dominates photocarrier be absorbed for suitable processing. The composite collection. We will measure the I-V characteristics and materials are formed into a paper with minor additions investigate the energy efficiencies for GaAs/AIGaAs and of cellulose using standard paper-making technology. InGaAs/lnP MQW solar cells with different well and Subsequent heating in a reducing atmosphere removes barrier configurations to select the best one. We will the cellulose and carbon, and forms essentially a pure study multi-unit GaAs-and InP-based MQW solar cells metallic shell, mimicking the size of the activated to further increase the range of the band gaps and the carbon precursor. The final dimensions of the rare earth energy efficiency. The target for the energy efficiency oxide fiber are determined by the initial dimensions of improvement is at least 150% for MQW solar cells over the precursor material. Successful samples will be the conventional bulk solar cells. Industrial evaluations characterized for strength, flexibility, and lifetime at will be made by two companies (Applied Solar Energy temperature. Large area radiators for specific in California and Plasma Physics in New York) during

119 Office of Energy Research

this project to determine the scientific and commercial where lattice mismatch produces recombination- potential of the MQW solar cells. promoting interface states.

Keywords: Solar Cells, Photovoltaic, Quantum Well, Keywords: Solar Cells, Photovoltaics, MOMBE, GaAs/AIGaAs, InGaAs/lnP Metalorganic Molecular Beam Epitaxy

269. A NOVEL TANDEM HOMOJUNCTION SOLAR 270. MAGNETICALLY ENHANCED CELL: AN ADVANCED TECHNOLOGY FOR THERMOELECTRIC COOLING HIGH EFFICIENCY PHOTOVOLTAICS $250,000 $255,000 DOE Contact: Walter M. Polansky, 301/903-5995 DOE Contact: Walter M. Polansky, 301/903-5995 Los Alamos National Laboratory Contact: Colorado State University Contact: Albert Migliori, 505/667-2515 Bruce Parkinson, 970/491-0504 Cryogenic solid-state refrigerators based on the A material for the construction of a solar cell must meet Ettinghausen effect can provide vastly superior a number of criteria to be suitable for large scale performance to Peltier devices, opening up new markets photovoltaic applications. It must be made up of in electronics and in superconductor-, and medical abundant elements, which are environmentally benign, applications. Surprisingly, this most effective of solid- and when combined into a crystal have suitable state cryogenic refrigeration processes is not being electronic properties. The required electronic properties studied at present. Yet it is much less restrictive in the include a bandgap in the 1.1-1.8 eV range, high possible materials that can be used, is simpler to absorption coefficients to minimize the amount of construct (even noting that a small permanent magnet material required, and high mobilities of photo must produce a field at the device), and has already generated carriers to facilitate the collection of these achieved lower temperatures than Peltier coolers, the carriers. The semiconductor, ZnSnP2, meets all of the only devices presently under investigation. Recent above requirements. It is isoelectronic with the III-V discoveries of new hybridization-gap semi-conductors alloy InGaP2, but has the advantage, for photovoltaic and semi-metals, and the commercial availability of applications, of not containing expensive and rare group high-strength Nd2Fe,4B permanent magnets, open the III elements. In addition, this material does not contain way for development of new ultra-high-performance, all toxic heavy metals such as are found in CdTe and solid-state Ettinghausen refrigerators. We will initiate CulnSe2/CdS thin film solar cells. The absorption studies of such coolers using modern materials to coefficient for this material is also very high. The engineer the world's best solid-state cryocooler. bandgap of ZnSnP2 has the additional interesting and useful property of ranging from 1.24 to 1.66 eV, Keywords: Thermoelectric Cooling, Peltier Devices, depending on the preparation conditions. Bulk crystal Solid-State Refrigeration, Ettinhausen growth techniques have not yielded high mobility Effect ZnSnP2 but there is no a prioni reason that the electronic properties of these materials cannot be as good as III-V 271. PHOTOCHEMICAL SOLAR CELLS materials, since very high mobilities were only achieved $150,000 in IIl-Vs after the development of modern epitaxial DOE Contact: Walter M. Polansky, 301/903-5995 growth techniques. State-of-the-art metal-organic National Renewable Energy Laboratory Contact: molecular beam epitaxy (MOMBE) will be used to grow Arthur J. Nozik, 303/384-6603 epitaxial layers of ZnSnP2 on lattice matched GaAs substrates. Studies of the order-disorder transition in Very high power conversion efficiencies (8-12%) for the metal sublattice, using both optical and electrical photochemical solar cells were reported in 1991. These techniques and especially solid state NMR to examine solar cells consist of highly porous nanocrystalline films atomic scale local environments, will be conducted in of TiO2 (band gap=3.0 eV) that are sensitized to the order to find the conditions for preparing materials with visible region of the solar spectrum through adsorption various bandgap energies and to understand the basic of Ru-containing metal-organic dye complexes on the chemistry and physics associated with this interesting TiO2 particle surface. This represents more than two order/disorder phase transition. When the conditions orders of magnitude improvement in the power are established for preparing a material of a given conversion efficiency of dye-sensitized semiconductor bandgap, a "tandem homojunction" solar cell will be electrodes in a photochemical cell. A dye-sensitized fabricated by variation of growth conditions in the photochemical solar cell system based on TiO2 powders MOMBE chamber in the appropriate way. This device- is very attractive from the point of view of potential low should show significant efficiency advantages over a cost and high semiconductor photo stability. This single material device or tandem heterojunction devices project is an integrated program of basic and applied development research that is funded jointly by three U.S. Department of Energy program offices: the

120 Office of Energy Research

Division of Chemical Sciences in the Office of Basic devoted to realization of a prototype device in which Energy Sciences, the Photovoltaic program in the Office either vertical-cavity surface-emitting laser structure or of Utility Technology and Advanced Energy Projects. In a pn junction is used to excite up-conversion addition to the molecular dye-sensitized TiO2 system, luminescence. research is also occurring to study other organic heterojunctions with wide bandgap semiconductors for Keywords: Light Emitting Diodes, GaAs, AIGaAs, photovoltaic applications. The AEP portion of the project GalnP2, AIGalnP2 , Energy Up Conversion, is to develop a configuration where the system is able to LED efficiently split water into hydrogen and oxygen, rather than to produce electricity. An inexpensive source of 273. ELECTRICALLY ACTIVE LIQUID MATRIX solar-produced hydrogen would be greatly beneficial to COMPOSITES the energy economy of the world, and would result in $300,000 the use of hydrogen as a non-polluting substitute for DOE Contact: Walter M. Polansky, 3011903-5995 many of the fuels currently in use. Oak Ridge National Laboratory Contact: Robert J. Lauf, 423/574-5176 Keywords: Photochemical Solar Cells, Hydrogen Production, Dye-Sensitive Semiconductors Varistors are nonlinear electrical resistors used to protect electrical equipment from the damaging effects 272. EFFICIENT ENERGY UP-CONVERSION OF of power surges. ZnO varistors are made by standard INFRARED TO VISIBLE LIGHT AT ceramic processes and are generally formed into SEMICONDUCTOR HETEROJUNCTIONS cylinders or disks electroded on the end faces. Failure $268,000 modes include catastrophic fracture, thermal runaway, DOE Contact: Walter M. Polansky, 301/903-5995 and slow degradation of electrical properties. 'Moldable' National Renewable Energy Laboratory Contact: surge protective materials, comprising metal and Hyeonsik M. Cheong, 303/384-6484 semiconductor particles dispersed in a silicone rubber matrix, are not as nonlinear as ZnO but can be formed A recently-discovered energy up-conversion into a number of devices by injection molding. -The phenomenon in semiconductor heterostructures will be material fails when an arc punches through at one point, studied. This phenomenon could be used to make light leaving a carbonized, conductive path to ground. We emitting devices that emit a wide range of colors and have recently discovered that a slurry of metal, even multiple colors or white light. Possible applications insulating, and semiconducting particles in dielectric oil for such devices are energy-efficient multi-color displays can exhibit the same nonlinearity as the moldable or a white light source to replace incandescent lamps in rubber compositions, but with the added features that it some areas. The principal advantage of such devices is self-healing, thixotropic, and its I-V characteristics would be that multiple elements of these up-conversion can serve as an excellent model system with which to structures with different emission colors, as well as the study the poorly-understood electrical phenomena that excitation source for the up-conversion, can be grown occur in moldable varistors. In this project, we will: monolithically on a single wafer. When GaAs/AIGalnP2 (1) determine the compositional limits for optimal heterostructures are excited with a near-infrared laser at electrical properties and relate these findings to 1.52 eV (815 nm), electrons and holes are created in theoretical percolation models; (2) determine the the lower-band-gap material (GaAs). Some of these rheological properties of the experimental materials and electrons and holes are excited to the higher-band-gap identify promising avenues for improving them; and material (AIGalnP2), and then radiatively recombine at (3) determine the dielectric constants and the the band gap of AIGalnP2, giving up-converted temperature dependence of key electrical properties. luminescence in red, orange, or green depending on the aluminum concentration in the AIGalnP2 alloy. The Keywords: Liquid Matrix Composites, Surge objective of the study is to demonstrate the feasibility of Protectors, Varistors, ZnO the devices utilizing this novel phenomenon of up- conversion. In order to achieve this, we will examine 274. SEMICONDUCTOR BROADBAND LIGHT various semiconductor heterostructures to find the EMITTERS optimal semiconductor heterostructure system that give $390,000 the highest up-conversion efficiency. This will require DOE Contact: Walter M. Polansky, 301/903-5995 sophisticated band-structure engineering using a Sandia National Laboratory Contact: number of different semiconductors including GaAs, Paul Gourley, 505/844-5806 AIGaAs, GalnP2, and AIGalnP2. We will also perform a systematic study of the mechanism for this up- Semiconductors are compact, lightweight, operate in conversion using both cw and ultrafast optical air, and are rugged. However, conventional semi- spectroscopies. The final phase of this project will be conductor diodes emit light only in a narrow range of

121 Office of Energy Research

wavelengths. To obtain broadband emission, new multi-disciplinary approach to synthesis and processing, structures are needed that utilize a wide range of alloy microstructural, thermomechanical and electrical compositions available from modern semiconductor investigation of select compositions around Mo5Si3B is growth techniques. Fractal lattice and chirped quantum being pursued. The investigation will focus on wells form a new class of materials which can provide establishing the fundamental relationship between broadband light emitters. The goal of this project is to composition, microstructure, and physical properties of develop such multi-alloy structures grown by metal B-doped Mo5Si3. In particular, select compositions will organic vapor phase epitaxy and molecular beam be synthesized and sintered to produce dense parts. A epitaxy for efficient, broadband light emission. To number of compositions will be studied for their stability develop broadband emitters, we will focus our efforts on in air and in corrosive atmospheres up to 1500°C. this class of fractal and chirped quantum-well structures Thermomechanical properties of successful conposi- utilizing InAIGaP alloys grown by metal-organic vapor tions will be investigated as a function of temperature phase epitaxy on GaAs substrates. The work will and will be related to their microstructure. Thermo- concentrate on three areas: materials design and electric properties such as thermal and electrical growth, characterization and modeling, and device conductivity will be determined at temperatures up to design and fabrication. The interplay of these three 1500°C and above. Optimum compositions will be parallel efforts will lead to optimized device structures determined and process scale-up will be considered for that emit broadband light with at least 300 meV heating element and heat exchanger applications. bandwidth in the green to red regions and a few percent external quantum efficiency. Materials and design Keywords: Heating Elements, Resistance Heaters, parameters will be understood through a wide variety of High Temperature Materials, MoSi2, experimental and theoretical tools. To implement this MosSi3B new class of broadband emitters, we will design, grow and fabricate light-emitting diode structures, and 276. PHOTOREFRACTIVE LIQUID CRYSTALS: measure electro luminescence spectra, current-voltage, NEW MATERIALS FOR ENERGY-EFFICIENT and light-current characteristics. IMAGING TECHNOLOGY $289,000 Keywords: Broadband Light Emitters, Indium- DOE Contact: Walter M. Polansky, 301/903-5995 Aluminum-Gallium-Phosphide, Fractal Argonne National Laboratory Contact: Lattice and Chirped Quantum Wells Gary P. Wiederrecht, 630/252-6963

MATERIALS PREPARATION, SYNTHESIS, This project will develop a new class of materials that DEPOSITION, GROWTH OR FORMING will be used to produce energy-efficient image processing micro-devices. These materials will exploit 275. NEXT GENERATION HIGH-TEMPERATURE the photorefractive effect, a light-induced change in the STRUCTURAL MATERIALS FOR HEAT refractive index of a nonlinear optical material that EXCHANGERS AND HEATING ELEMENTS results from photo generation of a space charge field $294,000 caused by directional charge transport over macro- DOE Contact: Walter M. Polansky, 301/903-5995 scopic distances within a solid. Both frequency and Ames Laboratory Contact: Mufit Akinc, phase information contained in light that has passed 515/294-0744 through a distorting medium can be recovered noise- free using photorefractive materials. The only high The project is centered on the development of a new quality photorefractive materials commercially available generation of electrical furnace heating elements and today are expensive single crystals of inorganic heat exchangers. Existing materials for heat exchangers materials such as barium titanate. This project will and heating elements are limited by their mechanical develop a completely new approach that combines and/or oxidative stability at high temperatures. MoSi 2 is cheap, easily processed organic materials with a built-in limited by its low creep strength above 1000°C whereas method of achieving the solid state order necessary to other metallic or intermetallic materials are limited to achieve photo refractivity comparable to that seen in about 1000°C. Increasing the temperature capability of inorganic crystals. The new approach uses organic existing heat exchangers and heating elements by molecules that undergo a phase transition above several hundred degrees and/or providing alternative ambient temperatures to a liquid crystalline phase. Self- furnace designs will provide significant energy ordering in the liquid crystalline phase, followed by efficiencies as well as ecological benefits. Recent work cooling to an ordered molecular solid, will impart both in our laboratory shows that boron doped Mo5Si3 good optical nonlinearity and directional photocon- exhibits outstanding oxidative stability in addition to its ductivity to thin solid films of these materials. These excellent high temperature creep strength and high solid films have the potential to possess greater melting point. However, a number of scientific and photorefractive sensitivity and faster response times technical issues remain to be elucidated. An integrated than any material developed to date. The liquid crystals

122 Office of Energy Research

will be based on easily oxidized, disc-shaped organic 278. SUPPORTED MOLTEN METAL CATALYSTS: molecules that are known to have liquid crystalline DEVELOPMENT OF A NEW CLASS OF phases. The specific materials will be derivatives of CATALYSTS triphenylenes, coronenes, porphyrins, and $322,000 phthalocyanines. These molecules can be used to DOE Contact: Walter M. Polansky, 301/903-5995 achieve the macroscopic order and good photoinduced University of Iowa Contact: Ravindra Datta, charge generation characteristics that are required of 319/335-1395 high quality photorefractive materials for application throughout the visible and near-infrared spectral This project is concerned with the design and regions. Intrinsically asymmetric, nonlinear optical development of an entirely novel class of active and molecules, e.g., a chiral p-nitroaniline derivative, will be selective catalysts called supported molten-metal attached to the disc-shaped molecules and oriented in catalysts (SMMC), with a view to eventually replace the liquid crystalline phase so as to maximize the some of the existing precious metal heterogeneous nonlinear susceptibility of the material. Optical studies catalysts used in the production of fuels and chemicals. on the resulting solids will be utilized to verify the SMMC is based on supporting ultra-thin films of the existence of photo refractivity and to accurately relatively low-melting, inexpensive, and abundant characterize the materials. Several device applications metals and semimetals, from groups la, lib, IlIb, IVb, will be demonstrated. Vb, and VIb elements, on porous refractory supports, much like supported microcrystallites of traditional solid Keywords: Photorefractive Liquid Crystals, Image catalysts. This technique could conceivably provide Processing, Nonlinear Optical Materials orders of magnitude higher surface area than that obtainable in conventional reactors containing molten 277. TRITIATED POROUS SILICON: A STAND- metals in pool form while avoiding corrosion. These ALONE POWER SOURCE have so far been the chief stumbling blocks in the use of $250,000 molten metal catalysts despite their higher selectivity DOE Contact: Walter M. Polansky, 301/903-5995 and lower susceptibility to deactivation. While the Argonne National Laboratory Contact: SMMC technique can be applied to a large variety of Carl E. Johnson, 630/252-7533 reactions, we will initially concentrate on dehydrogenation and reforming reactions due to their Tritiated porous silicon could form the basis for a new commercial significance. Thus, dehydrogenation of class of stand-alone power sources that are rugged and methylcyclohexane and decalin and reforming of portable and have high reliability over a very long period methylcyclopentane will be studied. These represent (>10 yr.). The tritium is covalently bonded to the silicon reactions of increasing complexity in catalytic reforming. and, thus, cannot escape as a gas into the environment. The initial choice is tellurium-based catalysts including This material would be able to provide the relatively low- alloys, due to the very promising results obtained in level power requirement of many types of highly preliminary screening experiments. Other catalytic integrated devices in optoelectronics and sensor formulations will also be tested. The activity, selectivity, technology. The proposed research involves three and stability of the selected catalysts will be compared tasks: (1) demonstrate the synthesis of tritiated porous with the traditional Pt catalyst in differential packed-bed silicon; (2) model the synthesis process; and (3) assess reactors. The commercial potential of the developed the optical activity of this novel material. The objective catalysts will be explored. of this project is to attain proof-of-concept and lay the foundation for development of a commercial device. Keywords: Molten Metal Catalysts, SMMC, The data base resulting from the proposed work would Dehydrogenation, Reforming provide a firm foundation for future engineering design efforts aimed at device development for specific 279. COMBINATORIAL SYNTHESIS OF HIGH T, applications. SUPERCONDUCTORS $250,000 Keywords: Porous Silicon, Power Supplies, Tritium DOE Contact: Walter M. Polansky, 301/903-5995 Lawrence Berkeley National Laboratory: X. D. Xiang, 510/486-6640

Currently, there is a tremendous interest in materials such as high temperature superconductors, organic conductors, permanent magnets, nonlinear optical materials and zeolites. However, even though the properties of such materials have been extensively investigated, few general principles have emerged that

123 Office of Energy Research allow one to predict the structures of new materials with will also be used. Essential to this project is a new enhanced properties. Consequently, the discovery of technique for fabricating micro-scale ferromagnetic such materials remains a time consuming and rather features. Organometallic chemical vapor deposition unpredictable trial and error process made even more techniques sufficient to deposit pure metal features with difficult by the increasing complexity of modern excellent spacial resolution have been developed at this materials. The question arises whether there is a more laboratory. These techniques allow selective deposition efficient and systematic approach to search through the of large uniform arrays of nickel, cobalt, cobalt- largely unexplored universe of ternary, quaternary, and palladium alloys and cobalt-palladium heterostructures higher order solid state compounds, in order to discover in features as small as 0.2 microns, and as thin as a materials with novel electronic, optical, magnetic or few monolayers or as thick as 10 microns. Multi layers mechanical properties. We will develop a new approach can be made by the successive deposition of different to materials discovery that will significantly increase the metals or alloys by the sequential photolysis of different rate at which novel materials are discovered as well as organometallic source compounds. While unconven- increase our ability to correlate physical properties with tional in many respects, this project utilizes a structure. Specifically, we will develop the ability to technology that is compatible with the fabrication of rapidly synthesize and analyze large libraries, or metal features 100 angstroms across in one Scanning- collections, of solid state materials for specific Tunneling microscopy run. The approach is superior to electronic, magnetic, optical and structural properties. techniques employing ion beams or conventional The aim of this project is twofold: (1) to develop the lithography and is inexpensive and compatible'with the technology to the point where it can be used effectively fabrication of the next generation of optical and for materials discovery; and (2) to apply the technology magnetic recording media. to the discovery of new superconducting materials. Keywords: Ferromagnetic Features, Micron-Scale Keywords: Combinatorial Synthesis, High Magnets, Organometallic CVD Temperature Superconductors, High Tc Superconductors, Superconducting 281. MICRO-HOLLOW CATHODE DISCHARGE Materials ARRAYS: HIGH PRESSURE, NONTHERMAL PLASMA SOURCES 280. FABRICATION AND CHARACTERIZATION OF $259,000 MICRON SCALE FERROMAGNETIC DOE Contact: Walter M. Polansky, 301/903-5995 FEATURES Old Dominion University Contact: $106,000 Karl H. Schoenbach, 757/683-4625 DOE Contact: Walter M. Polansky, 301/903-5995 University of Nebraska Contact: Hollow cathode discharges are known as nonthermal Peter A. Dowben, 402/472-9838 plasma sources: the electron energy distribution in the two stages of the discharge (predischarge and main This is a project to study micro scale features of discharge) contains a large percentage of high energy ferromagnetic nickel, cobalt, cobalt-palladium alloys (>10 eV) electrons. By reducing the size of the cathode and cobalt-palladium heterostructures fabricated by holes from cm to ten's of microns, we were able to "direct writing," i.e., by selective area deposition from extend their range of operation from subtorr range to organometallic compounds. There are two goals for this almost atmospheric pressure. The presence of high- research program. First, by making magnetic features energy electrons and the measured characteristics of smaller and smaller, in a variety of different shapes, the micro-hollow cathode discharges, such as: (1) positive project will elucidate the influence of defects on current voltage characteristics, which allow the magnetization reversal and coercivity. Second, the construction of discharge arrays without ballast, project will determine if there is any coupling between (2) stable operation for dc, ac, and pulsed voltages, small ferromagnetic features (approx. 1 micron), (3) low applied voltage (several hundred volts), and possibly substrate mediated, on the length scale of (4) strong radiative emission in the UV, allow the 1000 angstroms smaller. This research project is based utilization of micro-hollow cathode discharge arrays upon conventional methods for imaging magnetic (MHCDAs) for flat panel displays, surface processing, domains. Polarized light microscopy permits not only gaseous emission treatment, and as broad area imaging micron scale features but also determination of electron and ion sources. The MHCDAs consist either of the magnetic orientation and coercivity with some sets of metal meshes, spaced a distance on the order of spacial resolution. A microscope will be used to make the hole diameter apart, or of metal-plated, perforated polar Kerr rotation measurements and obtain spatially- dielectric foils. The simplicity, low cost, and the low selective magnetic information. A unique capability for required voltage for hollow electrode arrays makes probing the electronic structure of our magnetic features MHCDAs strong competitors to other electro- at resonance: spin polarized inverse photoemission technologies which rely on nonthermal plasmas (such with both longitudinal and transverse spin polarization as barrier discharges, and pulsed corona discharges).

124 Office of Energy Research

This project is studying the physics of micro-hollow with greatly improved energy efficiency and cost- cathode discharge operation in a positive differential effectiveness and will enable a significant reduction in conductivity mode. Particularly, the conditions for the use of heavy metal and solvent-based surface discharge array operation at atmospheric pressure are treatment coating processes. being explored, concentrating on the electron energy distribution and the spectral emission of micro-hollow Keywords: Ion Beam Processing, Rapid Solidification, cathode discharges. This project is focusing on two Surface Modification, Pulsed Ion Beams applications: (1) UV light sources (excimer lamps) for food and water sterilization and for surface treatment; 283. EXPERIMENTAL AND THEORETICAL and (2) gas reactors for treatment of hazardous gases, INVESTIGATION OF DUAL-LASER ABLATION such as perfluoro compounds, used in the FOR STOICHIOMETRIC LARGE-AREA semiconductor industry, and volatile organic MULTICOMPONENT FILM GROWTH compounds (VOC's). $108,000 DOE Contact: Walter M. Polansky, 301/903-5995 Keywords: Plasma Sources, Hollow-Cathode University of South Florida Contact: Discharge Sarath Witanachchi, 813/974-2789

282. RAPID MELT AND RESOLIDIFICATION OF We have recently discovered a novel dual-laser ablation SURFACE LAYERS USING INTENSE, PULSED process that dramatically alters the dynamics of the ION BEAMS conventional single-laser ablation process. Initial $300,000 experiments, using this process, allowed the production DOE Contact: Walter M. Polansky, 301/903-5995 of high quality, defect-free films of Y203 that were not Sandia National Laboratories Contact: possible with single excimer laser ablation. This Bob Turman, 505/845-7119 provided the motivation for investigating the physical mechanisms operative in this novel process. Two major In the past, the introduction of new material surface problems associated with single laser ablation have treatments like galvanizing, sputtering, and plasma hindered the development of this method as a spraying have enabled new products and opened new manufacturing process. They are: (1) deposition of markets. The capability to rapidly melt and resolidify micron and submicron particulates; and (2) relatively surface layers using intense, pulsed ion beams can narrow expansion profiles that limit the area of uniform enable another such advance. This project will develop film growth. Dual-laser ablation can potentially a next-generation surface processing technology based overcome both these major drawbacks while retaining on new, repetitively-pulsed ion beams. Rapid the main advantages of the single laser ablation solidification is known to greatly improve metal surface technique. A systematic study will be used to ascertain properties such as corrosion, wear, and fatigue expansion characteristics of individual elements, with resistance, but the lack of an economic and effective different volatility, in a multi-component material way to apply this technique to surfaces has prevented system, under the dual-laser ablation process that its use except in high value applications. Intense, would determine the required conditions for large-area pulsed, high energy ion beams treat surfaces through defect-free stoichiometric film growth. A species- surface melting followed by rapid thermal quenching by sensitive hydrodynamic model will be used. This will thermal diffusion into the underlying, untreated bulk provide a clear understanding of the basic mechanisms material. This process produces non-equilibrium micro- operative in this process, and thus aid the process structures, nanocrystalline phases, and extended solid optimization for any material system. The dual-laser solutions leading to improved corrosion and friction ablation system comprises a tandem combination of properties of metals, as well as surface smoothing and excimer and CO2 laser pulses with an adjustable inter- defect healing, grain refinement, and modification of pulse delay, that is spatially overlapped on the target. surface layer hardness. The low cost and in-depth The primary objective of the research is to study deposition of high energy pulsed ion beams gives experimentally the effect of the process parameters on pulsed ion beam technology important advantages over the species velocity distribution and expansion profile laser treatment. The project will determine the for individual components, and to develop a species- capabilities and limitations of rapid melt and sensitive theoretical model that is consistent with the resolidification using pulsed ion beams. It will document experimental observations. The project will investigate a the non-equilibrium micro-structures produced in treated Cu target to establish the process characteristics for a layers and their effect on metal surface properties and single-element plume. It will also study the expansion will do the initial process development needed to show characteristics of CulnSe2 and CulnxGaxSe2 plumes to how this technique can be applied to commonly used explore the behavior of individual elements in multi- metals. If successful, this will enable new ways to component plumes. Investigation of spatial modify surfaces for enhanced properties and lifetimes stoichiometric control of Ga in the Culn1,GaSe 2 will aid

125 Office of Energy Research semiconductor doping studies. The new understanding mechanical property envelope (including actual yield of the dual-laser ablation process will facilitate the and ultimate tensile strength measurements) and survey extension of this method to other material systems. The the corrosion resistance of this class of composites. method offers ease of control, simplicity and high- quality film growth, that could yield a method of choice Keywords: Shape Memory Alloy, Composite Materials, for both epitaxial and highly oriented polycrystalline Metal Matrix Composite multi-component film growth. 285. EXPLOITATION OF ROOM TEMPERATURE Keywords: Laser Ablation, Stoichiometric Evaporation, MOLECULE/ POLYMER MAGNETS FOR Dual Laser Ablation MAGNETIC AND ELECTROMAGNETIC INTERFERENCE SHIELDING AND MATERIALS PROPERTIES, BEHAVIOR, ELECTROMAGNETIC INDUCTION CHARACTERIZATION OR TESTING APPLICATIONS $212,000 284. SHAPE MEMORY ALLOY REINFORCEMENT DOE Contact: Walter M. Polansky, 301/903-5995 OF METALS Ohio State University: Arthur J. Epstein, $405,000 614/292-1133 DOE Contact: Walter M. Polansky, 301/903-5995 Oak Ridge National Laboratory Contact: There are increasing needs in today's society for Terry N. Tiegs, 423/574-5173 lightweight, electromagnetic radiation shielding materials for operation at low frequencies (

126 Office of Energy Research the study of the high Tc Prussian Blue-type magnetic electron diffraction will be used to characterize the materials, for shielding and induction applications from material surface after molecular debonding. The dc/low frequency to communications frequencies. The mechanistic understanding derived from these different objective of this project is to establish the ultimately techniques will be used to construct molecular achievable intrinsic real and imaginary magnetic frameworks that may provide corrosion resistance. The permeabilities and corresponding electric permittivities performance of these molecular architectures in real and their control through synthesis and processing. environments will be investigated using electrochemical reactors available at Exxon's Corporate Research Keywords: Polymer Magnets, Molecule-Based Laboratories. Magnets, Electromagnetic Shielding Keywords: Surface Modification, Corrosion Control, 286. MOLECULAR SURFACE MODIFICATION AS A Corrosion Inhibitors MEANS OF CORROSION CONTROL $292,000 SMALL BUSINESS INNOVATION RESEARCH DOE Contact: Walter M. Polansky, 301/903-5995 PROGRAM Princeton University Contact: Andrew B. Bocarsly, 609/258-3888 MATERIALS, PREPARATION, SYNTHESIS, DEPOSITION, GROWTH OR FORMING Corrosion is a major materials problem in many industries. In the petrochemical industry which provides PHASE I a major market for iron based materials, corrosion challenges exist from the production of hydrocarbons to Controlled Permeability Chemically Activated Fly Ash their refining and conversion to chemical products. (CAFA) for Reactive Contaminant Barrier - DOE Corrosion of concern to the petrochemical industry Contact Tom Hicks, (803) 725-2027; By-products occurs in a variety of environments ranging from highly Development Co. Contact Mr. Thomas Silverstrim, acidic to alkaline, and temperatures ranging from room (610) 461-2961 temperature up to -1100°C. The goal of this research is to investigate the chemistry of novel organic films Advanced Multilayer Braze foil for Si.N. Joining - DOE (corrosion inhibitors) of 5 angstroms to 20 angstroms Contact Yok Chen, (301) 903-3428; Eltron Research, dimension that may provide a corrosion resistant barrier Inc. Contact Ms. Eileen E. Sammells, (303) 440-8008 on the surface of metallic materials. Joint studies at Princeton University and Exxon Research and A Novel Reactive Joining Compound for High Engineering Company suggest that developments in the Temperature Applications - DOE Contact Yok Chen, fields of surface science and materials chemistry are (301) 903-3428; Sienna Technologies, Inc. Contact now at a point where an utilitarian molecular view of Dr. Ender Savrun, (425) 485-7272 corrosion processes is possible. This capability is expected to allow for the 'molecular design" of next Fabrication of Active Braze Alloys for High Temperature generation inhibitors having the requisite properties to Service - DOE Contact Yok Chen, (301) 903-3428; provide for corrosion protection under extreme chemical Surmet Corporation Contact Dr. Suri A. Sastri, and thermal conditions. In this project which is a (617) 272-3250 collaborative effort involving members of the Princeton Materials Institute and scientists from Exxon's Research Diamond-Like Nanocomposites: Hard. Wear Resistant. and Engineering Laboratory, state-of-the-art surface Low Friction Coatings for Triboloqical Applications - characterization tools will be brought together to DOE Contact Yok Chen, (301) 903-3428; Advanced generate a molecular level understanding of model Refractory Technologies, Inc. Contact Mr. Keith A organic films appropriate for corrosion control. The Blakely, (716) 875-4091 mechanisms of film protection and film breakdown will be investigated thoroughly. The order and packing High Growth Rate Cubic Boron Nitride Deposition - density of the films will be studied as a function of DOE Contact Yok Chen, (301) 903-3428; Applied temperature, using Grazing Incidence X-ray Diffraction Science And Technology, Inc. Contact involving synchrotron X-radiation as a main Mr. John M. Tarrh, (617) 937-5135 characterization tool. The interface stability of the molecule, its bonding mechanism and dissociation Development of Novel Boron-Based Multilaver pathways will be studied by using a combination of Thin-Film - DOE Contact Yok Chen, (301) 903-3428; spectroscopies such as Temperature Programmed Front Edge Technology, Inc. Contact Mr. Stephen Desorption, High Resolution Electron Energy Loss Denlinger, (818) 856-8979 Spectroscopy and Auger Electron Spectroscopy on model substrate surfaces. Additionally, low energy

127 Office of Energy Research

Nano-Lavered Diboride Materials with Enhanced Advanced Electrocatalysts for Direct Methanol Hardness. Strength. and Toughness for Wear Oxidation - DOE Contact JoAnn Milliken, Applications - DOE Contact Yok Chen, (301) 903-3428; (202) 586-2480; Giner, Inc. Contact Dr. Anthony B. Hyper-therm High-temperature Composites, Inc. LaConti, (617) 899-7270 Contact Mr. Wayne S. Steffier, (714) 375-4085 A Combinatorial Approach to the Synthesis and Advanced Plasma Surface Modification System - DOE Characterization of Novel Anode Materials for Direct Contact Yok Chen, (301) 903-3428; Ism Technologies, Methanol Fuel Cells - DOE Contact JoAnn Milliken, Inc. Contact Mr. Robert J. Stinner, (619) 530-2332 (202) 586-2480; Symyx Technologies Contact Mr. Isy Goldwasser, (408) 328-3100 High-Flux. Low Energy. Ion Source for High Rate Ion-Assisted Deposition of Hard Coatings - DOE Novel Multifunctional Direct Methanol Fuel Cell Contact Yok Chen, (301) 903-3428; Plasmaquest, Inc. Catalysts - DOE Contact JoAnn Milliken, Contact Dr. John E. Spencer, (972) 680-1811 (202) 586-2480; T/j Technologies, Inc. Contact Mr. Leslie Alexander, (313) 213-1637 An Ion Source Design Useful for the Production of Tribioloaical Thin Films - DOE Contact Yok Chen, Low Cost Deposition of Buffer Layers for (301) 903-3428; Stirling Technologies Inc. Contact Manufacturable YBCO HTS Conductors - DOE Contact Mrs. Bobbie C. Stirling, (423) 483-0142 James Daley, (202) 586-1165; American Supercon- ductor Corporation Contact Mr. Ramesh Ratan, Semi-Solid Thermal Transformation to Produce (508) 836-4200 Semi-Solid Formable Alloys - DOE Contact Yok Chen, (301) 903-3428; Hot Metal Molding, Inc. Contact Stoichiometric YBCO Epitaxial Coatings on RABITS Mr. B. Wilcox, (541) 298-0814 Using Low Cost CCVD Processing - DOE Contact James Daley, (202) 586-1165; Ccvd, Inc., Dba A Simple Process to Manufacture Grain Aligned Microcoating Technologies Contact Dr. Andrew T. Hunt, Permanent Magnets- DOE Contact Yok Chen, (770) 457-7767 (301) 903-3428; Advanced Materials Corporation Contact Mr. Vijay K. Chandhok, (412)268-5121 Buffer Layers on Textured Nickel Using Commercially Viable CCVD Processing - DOE Contact James Daley, A Novel Technigue for the Enhancement of Coercivitv in (202) 586-1165; Ccvd, Inc., Dba Microcoating High Enerya Permanent Magnets- DOE Contact Technologies Contact Mr. Jeffrey C. Moore, Yok Chen, (301) 903-3428; Advanced Materials (770) 457-7767 Corporation Contact Dr. S.G. Sankar, (412) 268-5649 Micromachined SiC Sensors For Harsh Environment Controlled Atmosphere Plasma Spraying of NdFeB Applications - DOE Contact Rolf Butters, Magnet Materials - DOE Contact Yok Chen, (202) 586-0984; Advanced Technology Materials, Inc. (301) 903-3428; Aps Material, Inc. Contact Mr. Joseph Contact Dr. Duncan W. Brown, (203) 794-1100 T. Cheng, (937) 278-6547 Silicon Carbide Sensors for Harsh Environments - DOE Stabilization of Nitride Magnet Material Via Sol-Gel Contact Rolf Butters, (202) 586-0984; Busek Company, Route - DOE Contact Yok Chen, (301) 903-3428; Inc. Contact Mrs. J. Budny, (508) 655-5565 Chemat Technology, Inc. Contact Ms. Jenny Sajoto, (818) 727-9786 Development of Efficient and Practical Passive Solar Building Systems with High Recycled Content Using the A Novel Process to Produce Nanostructured Permanent Preplaced Aggregate Concrete Technology - DOE Magnetic Materials - DOE Contact Yok Chen, Contact Mary Margaret Jenior, (202) 586-2998; Dpd, (301) 903-3428; Nanomaterials Research Corporation Inc. Contact Ms. Faragnis Jamzadeh, (517) 349-5653 Contact Dr. Tapesh Yadav, (520) 294-7115 Heterogeneous Hydroformylation of Alkanes with Coke Resistant Catalyst for the Partial Oxidation Synaas - DOE Contact Donald Krastman, Reforming of Hydrocarbon Fuels - DOE Contact (412) 892-4720; Tda Research, Inc. Contact JoAnn Milliken, (202) 586-2480; Aspen Systems, Inc. Mr. Michael E. Karpuk, (303) 940-2301 Contact Mr. Hamed Borhanian, (508) 481-5058 Advanced NZP-Ceramic Based Thermal Barrier CO Tolerant Doped-Metal Oxide Catalysts - DOE Coatings with Enhanced Oxidation and Thermal Shock Contact JoAnn Milliken, (202) 586-2480; Giner, Inc. Resistance - DOE Contact Udaya Rao, (412) 892-4743; Contact Dr. Anthony B. LaConti, (617) 899-7270 Lotec, Inc. Contact Mr. Santosh Y. Limaye, (801) 483-3100

128 Office of Energy Research

Tubular SOFC with Deposited Nano-Scale YSZ Epitaxial Growth of SiC on Silicon for Radiation Hard Electrolyte - DOE Contact Udaya Rao, Particle Detectors - DOE Contact Richard Piano, (412) 892-4743; Nextech Materials, Ltd. Contact (301) 903-4801; Lawrence Semiconductor Research Mr. William J. Dawson, (614) 766-4895 Laboratory, Inc. Contact Lamonte H. Lawrence, (602) 438-2300 Integrated Bandpass Filter Contacts for TPV Cells - DOE Contact Bill Barnett, (301) 903-3097; Edtek, Inc. Development of Scintillators and Waveshifters for Contact Mr. William E. Home, (206) 395-8084 Detection of Ionizing Radiation - DOE Contact Richard Plano, (301) 903-4801; Ludlum Measurements, In-Situ Ultrahigh-Pressure Wateriet Peening of Nuclear Inc. Contact Mr. Donald G. Ludlum, (915) 235-5494 Reactor Internals for the Prevention of Stress Corrosion Cracking - DOE Contact John Warren, (301) 903-6491; Low Viscosity Organic Insulation Systems For Improved Waterjet Technology, Inc. Contact Ms. Diana Suzuki, Processing and Reduced Radiation Induced Gas (206) 872-1925 Evolution - DOE Contact H. Stanley Staten, (301) 903-4950; Eltron Research, Inc. Contact Thallium-Containing III-V Quaternarv Compound Ms. Eileen E. Sammells, (303) 440-8008 Semiconductor for Use in Infrared Detection - DOE Contact Karl Veith, (202) 586-6002; Astropower, Inc. Radiation Resistant Joining Methods for Structural Contact Mr. Thomas J. Stiner, (302) 366-0400 Applications in Fusion Enerya Systems - DOE Contact F. W. Wiffen, (301) 903-4963; Starfire Systems, Inc. High Speed Long Wavelength Infrared Detector Contact Dr. Walter Sherwood, (518) 276-2112 Array/Preamplifier Development - DOE Contact Carl Friesen, (208) 526-1765; Fermionics Corporation PHASE II (FIRST YEAR) Contact Dr. Peter C.C. Wang, (805) 582-0155 An Attrition-Resistant Zinc Titante Sorbent for a Development of Cadmium Germanium Arsenide Transport Reactor - DOE Contact Daniel C. Cicero, Crystals - DOE Contact Carl Friesen, (304) 285-4826; Intercat Development, Inc. Contact Ms. (208) 526-1765; Inrad, Inc. Contact Mr. James L. Wendy L. Hansen, (908) 223-4644 Greco, 201-767-1910 A Light Scattering Based Sensor for On-Line Monitoring AllnGaN Light Emitting Diodes for Spectroscopic of Fiber Diameter Distribution During Fiberglass Applications - DOE Contact Carl Friesen, Manufacturing - DOE Contact Rolf Butters, (208) 526-1765; Svt Associates, Inc. Contact Dr. Peter (202) 586-0984; Mission Research Corporation Contact Chow, (612) 934-2100 Mr. Scot R. Fries, (805) 963-8761

An Easily Dispersed Reactive Coating for Surface Novel Use of Gas Jet Plasma to Prepare Amorphous Decontamination - DOE Contact Carl Friesen, Silicon Alloy - DOE Contact Alec Bulawka, (208) 526-1765; Lynntech, Inc. Contact Dr. Oliver J. (202) 586-5633; Energy Conversion Devices, Inc. Murphy, (409) 693-0017 Contact Ms. Nancy M. Bacon, (810) 280-1900 High Quantum Efficiency Spin-polarized High Rate Deposition of Transparent Conducting Zinc Photocathodes - DOE Contact Jerry Peters, Oxide Using Activated Oxygen for Photovoltaic (301) 903-5228; Spire Corporation Contact Mr. Richard Manufacturing Cost Reduction - DOE Contact S. Gregorio, (617) 275-6,000 Alec Bulawka, (202) 586-5633; Energy Photovoltaics, Inc. Contact Mr. David A. Jackson, (609) 587-3,000 Rapid Quench Nb3AI for High Field Accelerator Applications - DOE Contact Jerry Peters, Development of Optimal SnO, Contacts for CdTe (301) 903-5228; Plastronic, Inc. Contact Mr. Michael Photovoltaic Applications - DOE Contact Yok Chen, Tomsic, (937) 335-0656 (301) 903-3428; Green Development, LLC Contact Dr. Jianping Xi, (303) 278-4571 Ultra-Lightweight Carbon-Carbon Cooling Structure For Pixel and Silicon Strip Detectors - DOE Contact Large Area. Low Cost Processing for CIS Richard Plano, (301) 903-4801; Hytec, Inc. Contact Photovoltaics - DOE Contact Yok Chen, Mr. William O. Miller, (505) 662-0080 (301) 903-3428; International Solar Electric Technology, Inc. Contact Dr. Bulent Basol, (310) 216-4427

Improved Processes for Forming CIS Films - DOE Contact Yok Chen, (301) 903-3428; Unisun Contact Dr. Chris Eberspacher, (805) 499-7840

129 Office of Energy Research

Ultrafast Polvsilvlene Scintillators - DOE Contact Tim Low-Cost. Large-Area. Hiah-Resistivitv Substrates for Fitzsimmons, (301) 903-9830; Adherent Technologies, Gas Microstrip Detectors - DOE Contact Richard Meyer, Inc. Contact Ms. Susan K. Switzer, (505) 822-9186 (301) 903-3613; Spire Corporation Contact Mr. Richard S. Gregorio, (617) 275-6000 PHASE II (SECOND YEAR) An Economic Sorbent for the Removal of Mercury. Low Cost. Contamination-Tolerant Electrocatalvsts for Chlorine, and Hvdroaen Chloride from Coal Combustion Low-Temperature Fuel Cells - DOE Contact Flue Gases - DOE Contact Sean Plasynski, David Koegel, (301) 903-5997; Aspen Systems, Inc. (412) 892-4867; TDA Research, Inc. Contact Michael E. Contact Dr. Kang P. Lee, (508) 481-5058 Karpuk, (303) 940-2301

A Low Cost. High Temperature Superconductor Wire MATERIALS PROPERTIES, BEHAVIOR, Manufacturing Technology - DOE Contact James Daley, CHARACTERIZATION OR TESTING (202) 586-1165; American Superconductor Corporation Contact Mr. Ramesh Ratan, (508) 836-4200 PHASE I

A Low Cost Receiver Plate Manufacturing Process for Nondestructive Measurements of Key Mechanical High Concentration Photovoltaic Systems - DOE Properties of Alloy 718 Welded Structures Using Novel Contact Alec Bulawka, (202) 586-5633; Amonix, Inc. Stress-Strain Microprobe Technoloav - DOE Contact Contact Mr. Vahan Garboushian, (310) 325-8091 Yok Chen, (301) 903-3428; Advanced Technology Corporation Contact Mr. Fahmy M. Haggag, An Intumescent Mat Material for Joining of Ceramics to (423) 483-5756 Metals at High Temperatures - DOE Contact William J. Gwilliam, (304) 285-4401; CeraMem Corporation Processing For Surface Hardness: Novel Contact Dr. Robert L. Goldsmith, (617) 899-0467 Characterization Techniques for Dynamic Tribological Properties of Thin Films - DOE Contact Yok Chen, Development of Modulator Quality Rubidium Titanvl (301) 903-3428; Nano Instruments, Inc. Contact Arsenate Crystals for Remote Sensing Laser Systems - Dr. Warren C. Oliver, (423) 481-8454 DOE Contact Michael O'Connell, (202) 586-9311; Crystal Associates, Inc. Contact Mr. G. M. Loiacono, A Novel Mass Spectrometer for Characterization of (201) 612-0060 Electrochemical Processes - DOE Contact Al Landgrebe, (202) 586-1483; Southwest Sciences, A Novel Method to Recycle Thin Film Semiconductor Inc. Contact Mr. Alan C. Stanton, (505) 984-1322 Materials - DOE Contact Alec Bulawka, (202) 586-5633; Drinkard Metalox, Inc. Contact Mr. Fred Gallagher, New Insulation Techniques for High Voltage. High (704) 332-8173 Freauencv Motors - DOE Contact Jim Merritt, (202) 586-0903; Satcon Technology Corporation An Improved Material and Low-Cost Fabrication Contact Mr. David B. Eisenhaure, (617) 661-0540 Options for Candle Filters- DOE Contact William J. Gwilliam, (304) 285-4401; FluiDyne Engineering Development of Carbon Products from the Waste Corporation Contact Dr. Gary J. Hanus, (612) 544-2721 Stream of the Super Critical Deashing Process in Coal Liauefaction - DOE Contact Thomas Brown, An Integrated Catalyst/Collector Structure for (412) 892-4691; Fiber Materials, Inc. Contact Mr. David Regenerative Proton-Exchange Membrane Fuel Cells - R. Audie, (207) 282-5911 DOE Contact David Koegel, (301) 903-5997; Giner, Inc. Contact Dr. Anthony B. LaConti, (617) 899-7270 Sol-Gel Coatings as Corrosion Barriers for Carbonate Fuel Cell Components - DOE Contact Udaya Rao, Nanostructured Interstitial Alloys as Catalysts for Direct (412) 892-4743; Energy Research Corporation Contact Enerav Applications - DOE Contact David Koegel, (301) Mr. Hans C. Maru, (203) 825-6006 903-5997; Nanomaterials Research Corporation Contact Dr. Angelo Yializis, (602) 575-1354 Enhanced Flaw Detection by Time-Reversal Auto-Focusing of an Ultrasonic Array - DOE Contact Environmentally Responsible Recycling of Thin-Film John Warren, (301) 903-6491; Foster-Miller, Inc. Cadmium Telluride Modules - DOE Contact Alec Contact Mr. Adi R. Guzdar, (617) 684-4239 Bulawka, (202) 586-5633; Solar Cells, Inc. Contact Mr. Frederick L. Yocum, (419) 534-3377 High Resolution Cryogenic Calorimeter for Beta and Gamma Ray Detection - DOE Contact Dick Meyer, (301) 903-3613; Concept Technology Contact Dr. Alan Singsaas, (619) 695-0402

130 Office of Energy Research

High Current Density High Repetition Rate Ferroelectric Metal-Binding Silica Materials for Wastewater Cleanup - Cathode - DOE Contact Jerry Peters, (301) 903-5228; DOE Contact Kristine Bilenki, (301) 903-1687; Tpl, Inc. Fm Technologies, Inc. Contact Dr. Frederick M. Mako, Contact Ms. Jacqueline Taylor, (505) 343-8890 (703) 425-5111 Superhard Nanophase Cutter Materials for Rock Drilling High Current Capacity High Temperature Supercon- Applications - DOE Contact Paul Grabowski, ducting Film Based Tape for High Field Magnets - DOE (202) 586-0478; Diamond Materials, Inc. Contact Contact Jerry Peters, (301) 903-5228; Midwest Dr. Bernard H. Kear, (908) 445-2245 Superconductivity, Inc. Contact Dr. Jonathan W. Wilson, (913) 749-3613 Evaluation and Constitutive Modeling of Unidirectional SiC/SiC Composites with Engineered SiC Fiber A Polvcrvstalline Pixel Diamond Film Particle Detector- Coatings Subiected to Neutron Irradiation - DOE DOE Contact Richard Plano, (301) 903-4801; Applied Contact F. W. Wiffen, (301) 903-4963; Hyper-therm Science And Technology, Inc. Contact Mr. John M. High-temperature Composites, Inc. Contact Mr. Wayne Tarrh, (617) 937-5135 S Steffier, (714) 375-4085

Resistance Welding Vanadium Alloys - DOE Contact Innovative Fabrication of SiC/SiC Composites with High F. W. Wiffen, (301) 903-4963; Hitech Metallurgical Co. Through-the-Thickness Thermal Conductivity - DOE Contact Mr. Kenneth H. Holko, (619) 586-7272 Contact F. W. Wiffen, (301) 903-4963; Materials And Electrochemical Research (MER) Contact Dr. R. O. Low Cost Technigue for Testing Ceramic Insulator Loutfy, (520) 574-1980 Coatings - DOE Contact F. W. Wiffen, (301) 903-4963; Reb Research And Consulting Contact Dr. Robert E. High Numerical Aperture Scintillating Fibers - DOE Buxbaum, (810) 547-7942 Contact Robert Woods, (301) 903-3367; Biogeneral, Inc. Contact Ms. Andrea Gray, (619) 453-4451 PHASE II (FIRST YEAR) PHASE II (SECOND YEAR) Carbon Monoxide Tolerant Anodes for Proton Exchange Membrane (PEM) Fuel Cells - DOE Contact Ronald J. Rotating. In-Plane Magnetization and Magneto-Optic Fiskum, (202) 586-9154; EIC Laboratories, Inc. Contact Imaging of Cracks Under Coatings on Ferromagnetic Dr. A. C. Makrides, (617) 769-9450 Metals - DOE Contact Dennis Harrison, (301) 903-2884; Physical Research, Inc. Contact Dr. William C. L. Shih, Low Cost Advanced Bipolar Plates for Proton Exchange (310) 378-0056 Membrane Fuel Cells - DOE Contact Ronald J. Fiskum, (202) 586-9154; Materials And Electrochemical Development of Laser Materials and Ruaaed Coatings Research (MER) Contact Dr. J. C. Withers, as Components for Tunable Ultraviolet Laser Systems - (520) 574-1980 DOE Contact Michael O'Connell, (202) 586-9311; Lightning Optical Corporation Contact Mr. Wayne Improved Bi-2223 Flux Pinning Through Chemical Ignatuk, (813) 938-0092 Doping - DOE Contact James Daley, (202) 586-1165; American Superconductor Corporation Contact Application of Raman Spectroscopy to Identification and Mr. Ramesh Ratan, (508) 8364200 Sorting of Post-Consumer Plastics for Recycling - DOE Contact Simon Friedrich, (202) 586-6759; National Low Cost Multifilament Composite Process - DOE Recovery Technologies, Inc. Contact Dr. Charles E. Contact James Daley, (202) 586-1165; American Roos, (615) 734-6400 Superconductor Corporation Contact Mr. Ramesh Ratan, (508) 836-4200 A Sensor for Automated Plastics Sorting - DOE Contact Simon Friedrich,(202) 586-6759; Radiation Monitoring Template-Mediated Synthesis of Periodic Membranes Devices, Inc. Contact Dr. Gerald Entine, (617) 926-1167 for Improved Liguid-Phase Separations - DOE Contact Kristine Bilenki, (301) 903-1687; American Research Corporation Of Virginia Contact Mrs. Anne Churchill, (540) 731-0655

Novel Fiber-Based Adsorbent Technology - DOE Contact Kristine Bilenki, (301) 903-1687; Chemica Technologies, Inc. Contact Mr. Daniel J. Brose, (541) 385-0355

131 Office of Energy Research

DEVICE OR COMPONENT FABRICATION, Corrosion Resistant Bipolar Plates for PEM Fuel Cells - BEHAVIOR OR TESTING DOE Contact Jim Merritt, (202) 586-0903; Physical Sciences Inc. Contact Mr. George E. Caledonia, PHASE I (508) 689-0003

Hydrocarbon Gas Sensors Based on Wide Band-Gap Reduced Part Count Motor Fabrication - DOE Contact Semiconductors - DOE Contact Wanda Ferrell, Jim Merritt, (202) 586-0903; Unique Mobility, Inc. (301) 903-0043; Svt Associates, Inc. Contact Dr. Peter Contact Mr. Donald A French, (303) 278-2002 Chow, (612) 934-2100 Removal of Particulate and SOJNO, Precursors in Shaft Weld Replacement with a Ceramic Locking Integrated Gasification Combined Cycle Systems - DOE Assembly Joint - DOE Contact Yok Chen, Contact Mildred Perry, (412) 892-6015; Industrial Filter (301) 903-3428; Goss Engineers, Inc. Contact And Pump Manufacturing Company Contact Mr. Jeffrey Ms. Gabrielle M. Goss, (303) 721-8783 D. Burgeson, (708) 656-7800

A Novel Technology for Si3N,-To Superallov Joints With Use of Novel. Low-Cost Additives to Improve Sorbent High Use Temperature Capability - DOE Contact Yok Efficiency for Control of Mercury Emissions in Chen, (301) 903-3428; Materials And Electrochemical Coal-Fired Power Plant Flue Gases - DOE Contact Research (MER) Contact Dr. Raouf Loutfy, (520) Thomas Brown, (412) 892-4691; Physical Sciences Inc. 574-1980 Contact Mr. George E. Caledonia, (508) 689-0003

Development of Economical Procedures for Producing Mixed Phase Positive Electrodes for Long Life AMTEC and Processing Fine Grained SSM Feedstock via Modules - DOE Contact Bill Barnett, (301) 903-3097; Mechanical Stirring - DOE Contact Yok Chen, Tda Research, Inc. Contact Mr. Michael E. Karpuk, (301) 903-3428; Formcast, Inc. Contact Mr. Charles (303) 940-2301 Carlberg, (303) 778-6566 High Brightness LEDs Based on the (Al. Ga.ln)N A New Semi-Solid Forming Process For Fabrication of Materials System - DOE Contact Karl Veith, High Volume Fraction (>15 vol%) Metal/Metal Carbide (202) 586-6002; Advanced Technology Materials, Inc. Nanocomposites - DOE Contact Yok Chen, Contact Dr. Duncan W. Brown, (203) 794-1100 (301) 903-3428; Nanopowder Enterprises, Inc. Contact Dr. Gary S. Tompa, (908) 885-5909 Development of High Power RF Windows and Waveguide Components For the Next Linear Collider - Alternative Metal Forming Using Laser Engineered Net DOE Contact Jerry Peters, (301) 903-5228; Calabazas Shaping - DOE Contact Yok Chen, (301) 903-3428; Creek Research Contact Dr. R. Lawrence Ives, Optomec Design Company Contact Mr. Thomas A. (408) 741-8680 Swann, (505) 343-9139 Cost Reduction for Production of Superconducting Production of High Performance BSCCO-2223 Tapes Niobium Cavities - DOE Contact Jerry Peters, Using Hydrostatic Pressure - DOE Contact James (301) 903-5228; Meyer Tool & Mfg., Inc. Contact Daley, (202) 586-1165; American Superconductor Mr. Edward C. Bonnema, (708) 425-9080 Corporation Contact Mr. Ramesh Ratan, (508) 836-4200 Electrical Discharge Machining Application to the Development of mm-wave Accelerating Structures - Development of Long-length Fabrication Technology for DOE Contact Jerry Peters, (301) 903-5228; Ron High Tc Superconductors Operation in High Magnetic Witherspoon, Inc. Contact Dr. Steven Schwartzkopf, Fields at 77K - DOE Contact James Daley, (408) 370-6620 (202) 586-1165; Ues, Inc. Contact Mr. Francis F. Williams, Jr., (937) 426-6900 Direct Adhesive Technology for Arbitrary Conductors - DOE Contact Jerry Peters, (301) 903-5228; Advanced Non-Linear Inductor for Power Electronics Protection - Magnet Laboratory, Inc. Contact Mr. Mark W. Senti, DOE Contact Jim Merritt, (202) 586-0903; Energen, Inc. (407) 728-7543 Contact Dr. Chad H. Joshi, (617) 271-9876 Controlled Processing for High-Performance Fine Novel Fabrication of Low Cost Performance Bipolar Filament Bi-2223 Conductors - DOE Contact Jerry Plates - DOE Contact Jim Merritt, (202) 586-0903; Peters, (301) 903-5228; American Superconductor Materials And Electrochemical Research (MER) Contact Corporation Contact Mr. Ramesh Ratan, Dr. J. C. Withers, (520) 574-1980 (508) 836-4200

132 Office of Energy Research

Development of a High Field NbTi Superconductor Advanced Coal Based Power System Components Using an Approach Combining Artificial Flux Pinning Using Reaction Bonded Silicon Carbide - DOE Contact With Conventional Thermomechanical Processing - Otis Mills, (412) 892-5890; Busek Company, Inc. DOE Contact Jerry Peters, (301) 903-5228; Supercon, Contact Mrs. J. Budny, (508) 655-5565 Inc. Contact Ms. Elaine Drew, (508) 842-0174 A New Separation and Treatment Method for Soil and Conventionally Processed NbTi Superconductors with Groundwater Restoration - DOE Contact Kristine Artificial Ferromagnetic Pinning Centers for High Bilenki, (301) 903-1687; Lynntech, Inc. Contact Magnetic Field (>8 T) Application - DOE Contact Jerry Dr. Olive J. Murphy, (409) 693-0017 Peters, (301) 903-5228; Supercon, Inc. Contact Ms. Elaine Drew, (508) 842-0174 Continuous Analyzer for Monitoring Hvdrogen Chloride and Chlorine During Site Cleanup Activity - DOE Liquid Core Optical Scintillating Fibers - DOE Contact Contact Michael Torbert, (301) 903-7109; Ada Richard Piano, (301) 903-4801; Nano Systems, Inc. Technologies, Inc. Contact Dr. Judith Armstrong, Contact Mr. Robert W. Boerstler, (203) 881-2827 (303) 792-5615

High Performance Heat Pipe Cooling of Electron Long-Life Electrical Neutron Generator - DOE Contact Cyclotron Heating Mirrors P12-2426 - DOE Contact Michael O'Connell, (202) 586-9311; First Point T. V. George, (301) 903-4957; Thermacore, Inc. Scientific, Inc. Contact Dr. John R. Bayless, Contact Mr. Donald M. Ernst, (717) 569-6551 (818) 707-1131

Reaction Bonding of Silicon Carbide Composites for Passive Electronic Components from Nanostructured Fusion Applications - DOE Contact F. W. Wiffen, Materials - DOE Contact David Koegel, (301) 903-3159; (301) 903-4963; Busek Company, Inc. Contact Nanomaterials Research Corporation Contact Mrs. J. Budny, (508) 655-5565 Mr. Thomas Venable, (520) 294-7115

Net Shape Gradient W-Cu Plasma Facing Components A Multicore Optical Fiber Sensor for Mass Transport by Pressure Infiltration - DOE Contact Sam E. Berk, and Particulates - DOE Contact Wanda Ferrell, (301) 903-4171; Foster-miller, Inc. Contact Mr. Adi R. (301) 903-0043; Owen Research, Inc. Contact Mr. Brian Guzdar, (617) 684-4239 L. Sperry, (303) 427-1312

Joining of Silicon Carbide for Fusion Applications - DOE Infrared Hollow Waveguide Organic Solvent Analyzer - Contact F. W. Wiffen, (301) 903-4963; Lanxide DOE Contact Wanda Ferrell, (301) 903-0043; Polestar Corporation Contact Mr. Marc S. Newkirk, Technologies, Inc. Contact Ms. Karen K. Carpenter, (302) 456-6217 (617) 449-2284

A Novel Divertor Design Based on a Tungsten Wire Stratospheric Water Vapor Microsensor - DOE Contact Brush Tile - DOE Contact Sam E. Berk, (301) 903-4171; Wanda Ferrell, (301) 903-0043; Deacon Research Materials And Electrochemical Research (MER) Contact Contact Dr. Olive Lee, (415) 493-6100 Dr. Raouf O. Loutfy, (520) 574-1980 Compact. Airborne Laser Multigas Sensor - DOE Beryllium and Tunasten Brush Armor for Plasma Facing Contact Wanda Ferrell, (301) 903-0043; Physical Components - DOE Contact Sam E. Berk, Sciences, Inc. Contact Mr. George E. Caledonia, (301) 903-4171; Plasma Processes, Inc. Contact (508) 689-0003 Ms. Cheri McKechnie, (205) 851-7653 Microwave Radiometer for Passively and Remotely Fabrication for Reliable Tunasten Brush Structures for Measuring Atmospheric Water Vapor - DOE Contact Fusion Reactor Applications - DOE Contact Sam E. Wanda Ferrell, (301) 903-0043; Radiometrics Berk, (301) 903-4171; Surmet Corporation Contact Corporation Contact Dr. Randolph Ware, Dr. Suri A. Sastri, (617) 272-3250 (303) 497-8005

PHASE II (FIRST YEAR) Advanced Water Sensor for Unmanned Aerial Vehicles - DOE Contact Wanda Ferrell, (301) 903-0043; Catalytic Membrane for High Temperature Hvdroaen Southwest Sciences, Inc. Contact Dr. Alan C. Stanton, Separations - DOE Contact Otis Mills, (412) 892-5890; (505) 984-1322 Ceramem Corporation Contact Dr. Robert L. Goldsmith, (617) 899-0467 High-Gain Monocapillary Optics - DOE Contact Tim Fitzsimmons, (301) 903-9830; Aracor Contact Mr. Ed LeBaker, (408) 733-7780

133 Office of Energy Research

High Performance X-Rav and Neutron Microfocusing Coplanar CdZnTe p-l-n. Gamma-Ray Detectors for Optics - DOE Contact Tim Fitzsimmons, Nuclear Spectroscopy - DOE Contact Richard (301) 903-9830; Hirsch Scientific Contact Mr. Gregory Rinkenberger, (301) 903-3613; Spire Corporation Hirsch, (415) 359-3920 Contact Mr. Richard S. Gregorio, (617) 275-6000

Very Low Friction Small Radius Domed Cutters for Large Room Temperature Cd, Zn.. Detectors - DOE Percussion Drill Bits - DOE Contact Paul Grabowski, Contact Richard Rinkenberger, (301) 903-3613; W. (202) 586-0478; Novatek Contact Mr. David R. Hall, Peter Trower, Inc. Contact Dr. W. Peter Trower, (801) 374-6000 (540) 953-2249

Development and Testing of a Jet Assisted In-Situ Nondestructive Measurements of Key Polvcrystalline Diamond Drilling Bit - DOE Contact Paul Mechanical Properties of Reactor Pressure Vessels Grabowski, (202) 586-0478; Novatek Contact Mr. David Using Innovative SSM Technology - DOE Contact John R. Hall, (801) 374-6000 Warren, (301) 903-6491; Advanced Technology Corporation Contact Mr. Fahmy M. Haggag, Advanced Low-Stress Bonding of Thermally Stable (423) 483-5756 Polvcrvstalline Diamond Cutters to Tunasten Carbide Substrates - DOE Contact Paul Grabowski, Oxidation Induction Time Technoloav for Electric Cable (202) 586-0478; Science Research Laboratory, Inc. Condition Monitoring and Life-Assessment - DOE Contact Dr. Jonah Jacob, (617) 547-1122 Contact Dull Agarwal, (301) 903-3919; Pacific-sierra Research Corporation Contact Mr. Norman L. Duncan, Nanocrvstalline Superhard. Ductile Ceramic Coatings (703) 516-6372 for Roller Cone Bit Bearings - DOE Contact Paul Grabowski, (202) 586-0478; Spire Corporation Contact PHASE II (SECOND YEAR) Mr. Richard S Gregorio, (617) 275-6000 Advanced High Power Silicon Carbide Internally Cooled Solid-State Ultracapacitors for Electric Vehicles and X-Rav - DOE Contact Bill Oosterhuis, (301) 903-3426; Consumer Electronics - DOE Contact Al Landgrebe, SSG, Inc. Contact Mr. Dexter Wang, (617) 890-0204. (202) 586-1483; Cape Cod Research, Inc. Contact Ms. Katherine D. Finnegan, (508) 540-4400 Chemical Microsensor Arrays as Integrated Chip Compatible Devices for Chemical Weapons High Surface Area Non-Oxide Ceramic Electrodes for Nonproliferation Inspection - DOE Contact Robert Ultracapacitors - DOE Contact Al Landgrebe, Marianelli, (301) 903-5808; Microsensor Systems, Inc. (202) 586-1483; T/J Technologies, Inc. Contact Contact Dr. Hank Wohltjen, (502) 745-0099 Mr. Leslie Alexander, (313) 213-1637 A High Resolution Multi-hit Time to Digital Converter Wrappable Inorganic Electrical Insulators for Integrated Circuit - DOE Contact Robert Woods, Superconducting Magnets - DOE Contact T. V. George, (301) 903-3367; Lecroy Corporation Contact Mr. Joseph (301) 903-4957; Composite Technology Development, Migliozzi, (914) 578-6006 Inc. Contact Dr. Naseem A. Munshi, (303) 447-2226 A Helium-Cooled Faraday Shield Using Porous Metal Joining of Tunasten Armor Using Functional Gradients - Cooling - DOE Contact T. V. George, (301) 903-4957; DOE Contact T. V. George, (301) 903-4957; Plasma Thermacore, Inc. Contact Mr. Donald M. Ernst, Processes, Inc. Contact Ms. Cheri McKechnie, (717) 569-6551 (205) 851-7653 Low Cost Fabrication of Large Silicon Carbide/Silicon Carbon Thermostructure for Silicon-Based Particle Carbide Composite Structures - DOE Contact Detectors - DOE Contact Richard Piano, F. W. Wiffen, (301) 903-4963; Lanxide Corporation (301) 903-4801; Energy Science Laboratories, Inc. Contact Dr. Christopher Kennedy, (302) 456-6320 Contact Dr. Timothy R. Knowles, (619) 552-2034 Bandgap-Engineered Thermophotovoltaic Devices for High Performance Optical Detectors for Calorimetry - High Efficiency Radioisotope Power - DOE Contact DOE Contact Robert Woods, (301) 903-3367; Radiation Bill Barnett, (301) 903-3097; Edtek, Inc. Contact Monitoring Devices, Inc. Contact Dr. Gerald Entine, Mr. W. E. Home, (206) 395-8084 (617) 926-1167 Rugged. Tunable Infrared Laser Sources - DOE Contact Michael O'Connell, (202) 586-9311; Deacon Research Contact Dr. Olive Lee, (415) 493-6100

134 Office of Energy Research

An Innovative Membrane and Process for Removal and Low Loss Sapphire Windows for High Power Microwave Recovery of Natural Gas Liquids - DOE Contact Transmission - DOE Contact T V. George, William J. Gwilliam, (304) 285-4401; Membrane (301) 903-4957; Thoughtventions Unlimited Contact Technology And Research, Inc. Contact Dr. Stephen C. Bates, (203) 657-9014 Ms. E. G. Weiss, (415) 328-2228 DEVICE OR COMPONENT FABRICATION, A Lower Cost Molten Carbonate Matrix - DOE Contact BEHAVIOR OR TESTING William J. Gwilliam, (304) 285-4401; M-C Power Corporation Contact Mr. Patrick F. McSweeney, PHASE 1 (708) 986-8040 Novel Thin Film Scintillator for Intermediate Eneray SMALL BUSINESS TECHNOLOGY TRANSFER Photons Detection and Imaging - DOE Contact PROGRAM Dick Meyer, (301) 903-4398; NZ Applied Technologies, Inc. Contact Mr. Peter Norris, (617) 935-0300 MATERIALS PREPARATION, SYNTHESIS, DEPOSITION, GROWTH OR FORMING Silicon Carbide Heat Exchanger for Advanced Coal- Based Power Systems - DOE Contact Udaya Rao, PHASE I (412) 892-4743; Busek Company, Inc. Contact Dr. Vlad Hruby, (508) 655-5565 Improved Beta-Alumina Fabrication Using Rapid Plasma Sintering - DOE Contact David Koegel, Advanced Ceramic Hot Gas Filters - DOE Contact (301) 903-3159; Advanced Modular Power Systems, Theodore McMahon, (304) 285-4865; LoTec, Inc. Inc. Contact Dr. Thomas Hunt, (313) 677-4260 Contact Mr Santosh Y. Limaye, (801) 483-3100

New High-Performance GaSb-Based Thermo- PHASE II (FIRST YEAR) photovoltaic (TPV) Devices - DOE Contact David Koegel, (301) 903-3159; Astro Power, Inc. Contact High Speed Motor Alternators for Hybrid Electric Vehicle Dr. Allen Barnett (302) 366-0400 Eneryv Storage - DOE Contact Jim Merritt, (202) 586-0903, SatCon Technology Corporation High Efficiency Magnetic Refrigerators as Alternate Contract Mr. Michael Turmelle, (617) 349-0861 Environmentally Safe Commercial Refrigeration Devices - DOE Contact David Koegel, (301) 903-3159; A Flywheel Motor Alternator for Hybrid Electric Materials and Electrochemical Research Corp. Contact Vehicles - DOE Contact Jim Merritt, (202) 586-0903; Dr. R. O. Loutfy, (520) 574-1980 Visual Computing Systems Corporation Contact Mr. Robert J. Westerkamp, (812) 923-7474 PHASE II (FIRST YEAR) PHASE II (SECOND YEAR) Cabled Monofilament Subelements for Improved Multifilament Niobium Tin Performance and Reduced Environmentally Benign Manufacturing of Compact Disk Cost - DOE Contact Jerry Peters, (301) 903-5228; Stampers - DOE Contact Helen Kerch, (301) 903-2346; Supercon, Inc. Contact Ms. Elaine Drew, Prism Company Contact Mr. Peter Ciriello, (508) 842-0174 (508) 785-2511

PHASE II (SECOND YEAR) OFFICE OF FUSION ENERGY SCIENCES

Laser Processing of Thermal Sprayed Beryllium Plasma The mission of the Office of Fusion Energy Sciences Facing Components - DOE Contact T V. George, (OFES) is to advance plasma science, fusion science (301) 903-4957; Plasma Processes, Inc. Contact and fusion technology-the knowledge base needed for Mr. Tim McKechnie, (205) 851-7653 an economically and environmentally attractive fusion energy source. The policy goals that support this Amorphous Silicon/Crystalline Silicon Heteroiunctions mission are: (1) advance plasma science in pursuit of for Nuclear Radiation Detector Applications - DOE national science and technology goals; (2) develop Contact Richard Rinkenberger, (301) 903-3613; fusion science, technology and plasma confinement Quantrad Sensor, Inc. Contact Dr. Nicholas J. Szluk, innovations as the central theme of the domestic (408) 727-7827 program; and (3) pursue fusion energy science and technology as a partner in the international effort.

135 Office of Energy Research

A significant component of the fusion energy program is evaluating the response to irradiation conditions that the development and validation of the materials required simulate anticipated fusion system operation. The for the fusion systems. Materials must be developed compatibility studies include vanadium and other that will meet the unique requirements of fusion, as well candidate structural materials, and focus on the effects as the standard requirements of a high efficiency, high of exposure to projected coolants, including liquid reliability power generating system. The unique lithium and helium. requirements of fusion are the result of the intense neutron environment, dominated by the 14 MeV Keywords: Vanadium, Compatibility, Lithium, neutrons characteristic of the deuterium-tritium fusion Irradiation Effects, Alloy Development reaction. For performance, the materials must have slow and predictable degradation of properties in this 288. MODELING IRRADIATION EFFECTS IN neutron environment. For safety and environmental SOLIDS considerations, materials must be selected with $50,000 activation products that neither decay too rapidly DOE Contact: F. W. Wiffen, (301) 903-4963 (affecting such safety factors as system decay heat) nor LLNL Contact: T. Diaz de la Rubia, too slowly (affecting the waste management concerns (510) 422-6714 for end-of-life system components). Materials that meet these requirements are referred to as 'Low Activation Large scale computer simulation and experimental data Materials." Programs to develop the materials for on irradiation effects are combined to extend the plasma-facing components, for diagnostic and control understanding of the primary damage processes in systems, for structures in the high neutron flux regions, solids. Special attention is given to the energy range for the production of tritium in the blanket, and for the appropriate for the 14 MeV neutrons produced in D-T superconducting magnets required for confinement are fusion, and to the materials of interest for fusion sponsored by OFES. systems.

The fusion materials program in the United States is Keywords: Modeling, Irradiation Effects conducted with a high degree of international cooperation. Bilateral agreements with Japan and the 289. FUSION SYSTEMS MATERIALS Russian Federation enhance the ability of each party to $3,270,000 mount fission reactor irradiation experiments. The DOE Contact: F. W. Wiffen, (301) 903-4963 Fusion Materials Agreement under the International ORNL Contacts: E. E. Bloom, (423) 574-5053 Energy Agency (IEA) serves as a usefull venue for the and A. F. Rowcliffe, (423) 574-5057 exchange of information and the coordination of programs of research on Fusion Materials. Of particular This program is directed at the development and importance is the International Thermonuclear qualification of structural materials and insulating Experimental Reactor (ITER) engineering design ceramics for use in components of fusion power activity, conducted in partnership with the European systems exposed to the intense neutron flux. Candidate Union, Japan, and the Russian Federation. More than low activation structural material systems include one-half of the materials work sponsored by OFES is in ferritic/martensitic steels, vanadium alloys and SiC/SiC support of the ITER collaboration. composites. Investigations focus on the most critical questions or limiting properties in each of these MATERIALS PROPERTIES, BEHAVIOR, systems: ferritic/ martensitic steels-DBTT transition CHARACTERIZATION OR TESTING shifts and fracture toughness; vanadium alloys- welding processes, effects of irradiation on fracture 287. STRUCTURAL MATERIALS DEVELOPMENT toughness, and compatibility in proposed coolant $670,000 systems; SiC/SiC composites-definition of the effects DOE Contact: F. W. Wiffen (301) 903-4963 of irradiation on properties and structure and evaluation ANL Contact: D. L. Smith (630) 252-4837 of advanced composite fibers and coatings. The insulating ceramic activity is initially developing an This program is directed at the development of understanding of irradiation effects in alumina, spinel advanced, low activation structural materials for and other materials. The greatest concern is to establish application in fusion power system first wall and the permanent and transient changes in electrical blankets. Emphasis at ANL is on the development of properties, requiring measurement while the specimen vanadium-base alloys and on chemical corrosion/ is under irradiation. Work on these material classes compatibility of the structural materials with other involves irradiation in fission reactors, including HFIR, system materials. The vanadium alloy development is focused on the V-Cr-Ti system, with the goals of identifying promising candidate compositions, determining the properties of candidate alloys, and

136 Office of Energy Research

HFBR, and other test reactors, as partial simulation of with empirical data to develop physically-based models the fusion environment, of irradiation effects. The focus is on the fracture properties of vanadium alloys and ferritic stainless Keywords: Ceramics, Steels, Vanadium, Silicon steels, including helium effects, to: (a) develop an Carbide, Composites, Irradiation Effects, integrated approach to integrity assessment, Electrical Properties (b) develop advanced methods of measuring fracture properties, and (c) analyze the degradation of the 290. STRUCTURAL MATERIALS FOR FUSION mechanical properties of steels. The program also SYSTEMS contributes to the assessment of the feasibility of using $960,000 these alloys in ITER and other fusion systems. DOE Contact: F. W. Wiffen, (301) 903-4963 PNNL Contacts: R. H. Jones, (509) 376-4276 and Keywords: Vanadium, Steels, Irradiation Effects R. Kurtz, (509) 373-7515 Fracture

The goal of this program is to develop an understanding 293. DEVELOPMENT OF LITHIUM-BEARING of radiation effects that provides a basis for develop- CERAMIC MATERIALS FOR TRITIUM ment of irradiation-insensitive materials. The objective BREEDING IN FUSION REACTORS is low activation materials for use as structures in $100,000 divertor, first wall, and blanket components of fusion DOE Contact: S. Berk, (301) 903-4171 systems. Irradiation in fission reactors is used to ANL Contact: C. Johnson, (630) 252-7533 simulate fusion conditions, with measurement of physical and mechanical properties used to track Research activities are focused on critical issues of irradiation effects. A modeling activity complements the ceramic breeder blankets for fusion reactors, including experimental measurements. The ultimate goal is ceramic breeder material tritium retention and release, optimized ferritic steels, vanadium alloys, and SiC/SiC ceramic breeder and beryllium irradiation response, composite materials for fusion power plant use. chemical compatibility of ceramic breeder materials and beryllium with blanket coolant and structural materials, Keywords: Steels, Vanadium, Silicon Carbide, and heat transfer and temperature control in ceramic Composites, Irradiation Effects, Modeling breeder materials. Computer models are tested against data on irradiation of lithium-oxide and lithium-zirconate 291. DEVELOPMENT OF RADIATION-HARDENED materials in a fast-spectrum fission reactor. There is CERAMIC COMPOSITES FOR FUSION good agreement between model predictions and APPLICATIONS experimental data in the area of transient tritium $28,000 release. DOE Contact: F. W. Wiffen, (301) 903-4963 RPI Contact: D. Steiner, (518) 276-4016 Keywords: Ceramics, Compatibility, Tritium Release, Modeling, Lithium Ceramics This research is directed at furthering the understanding of the effects of irradiation on the SiC/SiC composite 294. POST-IRRADIATION EXAMINATION OF system, as the basis for developing superior composite LITHIUM-BEARING CERAMIC MATERIALS materials for fusion structural applications. The focus of FOR TRITIUM BREEDING IN FUSION the work is on the evaluation of improved fibers and REACTORS alternative interface layer materials. $20,000 DOE Contact: S. Berk, (301) 903-4171 Keywords: Silicon Carbide, Composites PNNL Contact: G. Hollenberg, (509) 376-5515

292. DAMAGE ANALYSIS AND FUNDAMENTAL Research activities are for post-irradiation examinations STUDIES FOR FUSION REACTOR MATERIALS (PIE) of the ceramic breeder materials irradiated in the DEVELOPMENT Fast Flux Test Facility. The PIE was conducted as part $150,000 of the BEATRIX-II program under an International DOE Contact: F. W. Wiffen, (301) 903-4963 Energy Agency agreement between the US, Japan and UCSB Contacts: G. R. Odette, (805) 893-3525 Canada. PIE involved capsule disassembly, neutron and G. E. Lucas, (805) 893-4069 radiography, plenum gas analysis, photography, mensuration characterization, tritium inventory This research is directed at developing a fundamental measurements, microstructural characterization and understanding of both the basic damage process and thermal conductivity measurements. PIE for specimens microstructural evolution that take place in a material from the BEATRIX-II Phase 1 irradiation (lithium-oxide during neutron irradiation. This understanding is used irradiated to 5 percent lithium atom burnup) and the

137 Office of Energy Research

Phase 2 irradition (lithium-oxide and lithium-zirconate emphasizes the use of the HFIR and of fission test irradiated to 5 percent lithium atom burnup) was reactors in Russia to perform the irradiations in support completed in FY 1995. of the ITER materials development and evaluation.

Keywords: Ceramics, Lithium Ceramics, Tritium Keywords: Steels, Copper, Vanadium, Ceramics, Release Irradiation Effects, Electrical Properties

295. INTERNATIONAL THERMONUCLEAR 297. ITER STRUCTURAL MATERIALS EVALUATION EXPERIMENTAL REACTOR (ITER) MATERIALS $200,000 DEVELOPMENT FOR PLASMA FACING DOE Contact: F.. Wiffen, (301) 903-4963 A S I A r A CING COMPONENTSCOMPONhENTS *- " PNNL Contact: R. H. Jones, (509) 376-4276 $5,000,000 Materials systems of interest to ITER for use as DOE Contact: S. Berk, (301) 903-4171 structural materials in the divertor, first wall and SNL Contact: M. Ulrickson, (505) 845-3020 blankets are under evaluation to select the most attractive candidates in each system, and to develop the Research activities include: improved techniques for property database on these. The PNNL program is joining beryllium or tungsten to copper alloys, deter- evaluating copper alloys and stainless steels for the mination of the tritium retention of beryllium, ITER program. The emphasis is on.irradiation effects, improvement of the thermal conductivity of plasma especially on fracture properties, for the bonded sprayed beryllium, development of radiation damage structures. resistant carbon-fiber composites, determination of erosion rates of beryllium, tungsten and carbon under Keywords: Steels, Copper, Irradiation Effects normal and disruption conditions and thermal fatigue testing of beryllium, tungsten and carbon-fiber 298. DEVELOPMENT OF Nb3Sn composites. The joining techniques being investigated SUPERCONDUCTING WIRE FOR THE ITER include diffusion bonding, induction brazing, MAGNET PROGRAM electroplating and inertial welding. Tritium retention and $200,000 permeation measurements have been conducted on the DOE Contact: T. V. George, (301) 9034957 Tritium Plasma Experiment. The improvements in the MIT Contact: J. Minervini, (617) 253-5503 plasma spray technique are centered on improving the beryllium powder and selection of the proper powder A major development and industrial procurement sizes. Highly oriented pitch based carbon fibers have activity of a high critical current density Nb3Sn been used to produce carbon-fiber composite for superconducting wire for use in the ITER Model Coil neutron irradiation. The erosion rates are measured on program was completed recently. Intermagnetics both plasma simulators and tokamaks. The thermal General Corporation/Advanced Superconductors Inc. fatigue testing is carried out on electron beam test (IGC/ASI) delivered over 5 metric tons of supercon- systems. ducting wire to the ITER HPI strand specification. The strand was subsequently cabled by BIW, Inc. into Keywords: Plasma-Facing Components, Beryllium, 4 cables of greater than 1000 strands, each over 200m Tungsten, Carbon-Fiber Composite, long, for use in the US Inner Coil Module of the ITER Joining, Erosion, Thermal Fatigue CS Model Coil. The strand procurement program was supported by characterization and acceptance 296. ITER MATERIALS EVALUATION measurements of strand critical superconducting $330,000 properties and ac losses by several university and DOE Contact: F. W. Wiffen, (301) 903-4963 national laboratories. Further work is continuing to ORNL Contacts: E. E. Bloom, (423) 574-5053 enhance the wire performance while reducing and A. F. Rowcliffe, (423) 574-5057 production costs.

ITER requires structural materials and insulating Keywords: Superconductors, Magnet Materials, Nb3Sn ceramics for use in a range of system components exposed to the neutrons produced by the fusion 299. STRUCTURAL MATERIALS DEVELOPMENT reaction. ORNL's part of the ITER materials program is FOR THE CONDUIT OF ITER directed at the selection of promising compositions of CABLE-IN-CONDUIT-CONDUCTORS copper alloys, evaluating bonded copper alloy-stainless $200,000 steel structures and assisting in the development of the DOE Contact: T. V. George, (301) 903-4957 database needed for the use of these materials. MIT Contact: J. Minervini, (617) 253-5503 Irradiation effects and mechanical properties of these materials are under study. The insulating ceramics work The conduit material selected for the ITER is focused on the electrical properties under irradiation, cable-in-conduit-conductors is the high strength and the in situ measurement techniques to determine superalloy Incoloy Alloy 908, developed via this response are being developed. The work at ORNL collaboration between INCO Alloys International (IAI)

138 Office of Energy Research and MIT. IAI has recently delivered over 60 metric tons of this material in the shape of square extrusions with a circular hole, in unit lengths up to 10m, for the ITER CS Model Coil Program. A significant database has been developed by materials properties characterization as well as industrial processing experience and coil winding experience. Work is continuing on alloy development to reduce the sensitivity of the material to Stress Accelerated Grain Boundary Oxidation (SAGBO). Keywords: Conduit, Incoloy, Magnet Materials

139 Office of Environmental Management

OFFICE OF ENVIRONMENTAL MANAGEMENT

FY 1997

Office of Environmental Management - Grand Total $6,870,939

Materials Properties, Behavior. Characterization or Testing $6,870,939

The Influence of Radiation and Multivalent Cation Additions on Phase Separation and Crystallization of Glass 241,000 Chemical and Ceramic Methods Toward Safe Storage of Actinides Using Monazite 429,000 Atmospheric-Pressure Plasma Cleaning of Contaminated Surfaces 404,000 Chemical Decomposition of High-level Nuclear Waste Storage/Disposal Glasses Under Irradiation 163,000 Analysis of Surface Leaching Processes in Vitrified High-Level Nuclear Wastes Using in situ Raman Imaging and Atomistic Modeling 186,333 Investigation of Microscopic Radiation Damage in Waste Forms Using ODNMR and AEM Techniques 232,667 in situ Spectro-Electrochemical Studies of Radionuclide Contaminated Surface Films on Metals and the Mechanism of their Formation and Dissolution 335,000 Determination of Transmutation Effects in Crystalline Waste Forms 304,328 Radiation Effects on Materials in the Near-Field of Nuclear Waste Repository 136,000 An Alternative Host Matrix Based on Iron Phosphate Glasses for the Vitrification of Specialized Nuclear Waste Forms 208,278 Microstructural Properties of High Level Waste Concentrates and Gels with Raman and Infrared Spectroscopies 155,000 Fundamental Thermodynamics of Actinide-Bearing Mineral Waste Forms 383,333 Photooxidation of Organic Wastes Using Semiconductor Nanoclusters 417,000 Optimization of Thermochemical, Kinetic, and Electrochemical Factors Governing Partitioning of Radionuclides During Melt Decontamination of Radioactively Contaminated Stainless Steel 400,000 Mechanism of Pitting Corrosion Prevention by Nitrite in Carbon Steel Exposed To Dilute Salt Solution 216,667 Stability of High-Level Waste Forms 254,000 Radiation Effects in Nuclear Waste Materials 960,000 New Silicotitanate Waste Forms: Development and Characterization 400,000 Ion-Exchange Processes and Mechanisms in Glasses 300,333 Distribution & Solubility of Radionuclides & Neutron Absorbers in Waste Forms for Disposition of Plutonium Ash & Scraps, Excess Plutonium, and Miscellaneous Spent Nuclear Fuels 600,000 Modeling of Diffusion of Plutonium in Other Metals and of Gaseous Species in Plutonium-Based Systems 145,000

140 Office of Environmental Management

OFFICE OF ENVIRONMENTAL MANAGEMENT

The Office of Environmental Management (EM) was established to effectively coordinate and manage the Department's activities to remediate the DOE Defense Complex and to properly manage waste generated by current operations. EM conducts materials research within two offices:

Office of Waste Management - The Office of Waste Management uses current technologies to minimize production of DOE-generated waste, alter current processes to reduce waste generation, and work with the Office of Science and Technology to develop innovative technologies for the treatment and disposal of present and future waste streams. The mission of the Office is to minimize, treat, store, and dispose of DOE waste to protect human health, safety, and the environment. Office of Science and Technoloav - The Office of Science and Technology (OST) is responsible for managing and directing targeted basic research and focused, solution-oriented technology development programs to support the DOE Office of Environmental Management (EM). Programs involve research, development, demonstration, and deployment activities that are designed to produce innovative technologies and technology systems to meet national needs for regulatory compliance, lower life-cycle costs, and reduced risks to both people and the environment. Certain areas of the OST program focus on materials research in order to provide better, safer and less expensive approaches to identify, characterize and remediate DOE's waste problem. Four Focus Areas have been formed to focus the EM-wide technology development activities on DOE's most pressing environmental management problems and are co-led by all EM offices:

Subsurface Contaminants. Hazardous and radioactive contaminants in soil and groundwater exist throughout the DOE complex, including radionuclides, heavy metals, and dense, nonaqueous phase liquids. Groundwater plumes have contaminated over 600 billion gallons of water and 50 million cubic meters of soil. In addition, the Subsurface Contaminants Focus Area is responsible for supplying technologies for the remediation of numerous landfills at DOE facilities. Technology developed within this speciality area provides effective methods to contain contaminant plumes and new or alternative technologies for remediating contaminated soils and groundwater.

Radioactive Tank Waste Remediation. Across the DOE Complex, hundreds of large storage tanks contain hundreds of thousands of cubic meters of high-level mixed waste. Primary areas of concern are deteriorating tank structures and consequent leakage of their contents. Research and technology development activities must focus on the development of safe, reliable, cost-effective methods of characterization, retrieval, treatment, and final disposal of the wastes.

Mixed Waste Characterization. Treatment, and Disposal. DOE faces major technical challenges in the management of low-level radioactive mixed waste. Several conflicting regulations together with a lack of definitive mixed waste treatment standards hamper mixed waste treatment and disposal. Disposal capacity for mixed waste is also expensive and severely limited. DOE now spends millions of dollars annually to store mixed waste because of the lack of accepted treatment technology and disposal capacity. In addition, currently available waste management practices require extensive, and hence costly waste characterization before disposal. Therefore, DOE must pursue technology that leads to better and less expensive characterization, retrieval, handling, treatment, and disposal of mixed waste. Decontamination and Decommissioning. The aging of DOE's weapons facilities, along with the reduction in nuclear weapons production, has resulted in a need to transition, decommission, deactivate, and dispose of numerous facilities contaminated with radionuclides and hazardous materials. While building and scrap materials at the sites are a potential resource, with a significant economic value, current regulations lack clear release standards. This indirectly discourages the recovery, recycling, and/or reuse of these resources. The development of enhanced technologies for the decontamination of these materials, and effective communication of the low relative risks involved, will facilitate the recovery, recycle, and/or reuse of these resources. Improved materials removal, handling, and processing technologies will enhance worker safety and reduce cost.

The projects listed in this report are managed under the Environmental Management Research Program (EMSP), a joint program of EM and the Office of Energy Research (ER). Basic research under the EMSP contributes to environmental management activities that decrease risk to the public and workers, provide opportunities for major cost reductions, reduce time required to achieve EM's mission goals, and, in general, address problems that are considered intractable without new knowledge. This program is designed to inspire 'breakthroughs' in areas critical to the EM mission through basic research and is managed in partnership with ER. ER's well-established procedures are used for merit review of applications to the EMSP. Subsequent to the formal scientific merit review, applications that are judged scientifically meritorious are evaluated by DOE for relevance to the objectives of the EMSP. The current EMSP portfolio consists of 202 awards amounting to a total of $160 million in three-year funding. Twenty-one of those awards were in scientific disciplines related to materials issues that have potential to solve Environmental Management challenges. The 1997

141 Office of Environmental Management component of materials research amounts to $6,870,939. This figure is smaller than that reported for FY96 because of a redefinition of the materials research component. The entire EMSP portfolio can be viewed on the World Wide Web at http://www. em. doe. gov/science.

MATERIALS PROPERTIES, BEHAVIOR, 301. CHEMICAL AND CERAMIC METHODS CHARACTERIZATION OR TESTING TOWARD SAFE STORAGE OF ACTINIDES USING MONAZITE 300. THE INFLUENCE OF RADIATION AND $429,000 MULTIVALENT CATION ADDITIONS ON PHASE DOE Contact: Chet Miller, (202) 586-3952 SEPARATION AND CRYSTALLIZATION OF Rockwell International Corporation Contact: GLASS P.E.D. Morgan, (805) 373-4273 $241,000 ORNL Contact: Lynn A. Boatner, DOE Contact: Chet Miller, (202) 586-3952 (423) 574-5492 University of Arizona Contact: Michael C. Weinberg, (520) 621-6909 The program is investigating monazite ceramics for safe, secure, geologically tested, very long term, Recent reviews which have dealt with critical issues containment for actinides. The main outstanding regarding the suitability of glasses for nuclear waste fundamental research issues facing the use of monazite disposal have identified liquid-liquid immiscibility and as a waste form necessitate the development of crystallization processes as having the potential to alter fundamental understanding of: sintering mechanisms significantly storage behavior, especially chemical involved in forming high density monazite ceramics; corrosion characteristics. These phase transformation physical and chemical properties of grain boundaries in processes can be abetted (or deterred) by radiation or these ceramics; interactions with impurities and the inclusion of small quantities of other components additives used to promote densification; physical such as transition metals, rare earths, actinides, etc. properties of polycrystalline monazite ceramics; and the Consequently, in order to minimize the chances for the precipitation of monazite phases in an efficient, simple occurrence of deleterious phase separation or and economical manner. This program is addressing crystallization, it is essential to examine the influence of these issues to serve as a knowledge base for using these factors on phase transformation kinetics. monazite as a nuclear waste form.

The major goal of this program is to study the influence Keywords: Monazite, Waste Form, Sintering, of irradiation and multivalent cations and redox Densification conditions upon the thermodynamics and kinetics of phase separation and crystallization in selected glass 302. ATMOSPHERIC-PRESSURE PLASMA compositions. Any observed changes in transformation CLEANING OF CONTAMINATED SURFACES behavior will be related to structural modifications $404,000 caused by radiation. Finally, guidelines will be DOE Contact: Chet Miller, (202) 586-3952 developed to mitigate the deleterious effects of phase University of California at Los Angeles separation and crystallization by composition Contact: Robert F. Hicks, (310) 206-6865 adjustments, based on the development of a database LANL Contact: Gary Selwyn, from ongoing and existing measurements and the (505) 667-7824 development of appropriate models. Decommissioning of transuranic waste (TRU) into The characteristics of phase separation are being low-level radioactive waste (LLW) represents the largest analyzed, experimentally, using SEM, EDS, HSEM, cleanup cost associated with the nuclear weapons TEM, and SAXS. Crystallization is being studied using complex. This project is developing a low-cost XRD, SEM, TEM, and optical microscopy. Structural technology for converting TRU into LLW based on the changes are being examined using IR and Raman selective plasma etching of plutonium and other Spectroscopies and solid state NMR measurements. actinides from contaminated structures. Plasma etching has already been used to remove Pu films from Keywords: Radiation, Phase Separation, materials. However, this process is operated under Crystallization, Glasses vacuum, making it both expensive and difficult to apply to many nuclear wastes. A major breakthrough in this field was the demonstration of the operation of a g-mode, resonant-cavity, atmospheric-pressure plasma jet (APPJ). This jet etches kapton at between 10 and 15 pm/hour, and tantalum at between 1 and 2 pJm/hour. Etching occurs below 373 K, so that delicate materials will not be destroyed by this process. The plasma jet may be used to selectively remove plutonium and other actinide elements by converting them into volatile compounds that are trapped by adsorption and filtration.

142 Office of Environmental Management

Since the jet operates outside a chamber, many nuclear 304. ANALYSIS OF SURFACE LEACHING wastes may be treated, including machinery, duct-work, PROCESSES IN VITRIFIED HIGH-LEVEL concrete and other building materials. At LANL, the NUCLEAR WASTES USING IN-SITU RAMAN source physics is being studied using Stark-broadening, IMAGING AND ATOMISTIC MODELING microwave interferometry, and laser-induced $186,333 fluorescence (LIF). The metastables, neutrals and DOE Contact: Chet Miller, (202) 586-3952 radical species produced with mixtures of NF3, CF4, University of Florida Contact: C2F6, 02,He and Ar are being identified by LIF, optical Joseph H. Simmons, (352) 3926679 emission spectroscopy (OES), laser Raman spectroscopy (LRS), coherent anti-Stokes Raman This research combines a novel investigative technique spectroscopy (CARS), and mass spectroscopy (MS). At with novel modeling studies to analyze leaching UCLA, the elementary surface reactions of these processes in glasses. Its utility is that it will provide both species with tantalum and tungsten (surrogate metals a means of conducting fundamental studies of the for Pu) are being studied in ultrahigh vacuum using a corrosion behavior of high valence and multivalent ions supersonic molecular-beam coupled to the plasma jet. in the waste glass as well as a proven in-situ method for The surfaces are being characterized by X-ray monitoring the chemical corrosion behavior of radio- photoemission (XPS), infrared spectroscopy (IR), active waste glasses, remotely and in burial sites. The low-energy electron diffraction (LEED), and research has three major thrusts: (1) the development scanning-tunneling microscopy (STM). In addition, of in-situ Raman Imaging Spectroscopy for a detailed plutonium etching experiments are being carried out at examination of leaching processes and associated the Los Alamos Plutonium Facility. structural changes and mineral precipitates on the surface of borosilicate glasses loaded with simulated Keywords: Plasma Etching, Plutonium high-level nuclear wastes, (2) the application of this method to the analysis of transition states and their 303. CHEMICAL DECOMPOSITION OF HIGH-LEVEL energetics during surface leaching by novel modeling NUCLEAR WASTE STORAGE/DISPOSAL studies, and by comparison with existing methods of IR, GLASSES UNDER IRRADIATION Auger XPS and SIMS spectroscopy, SEM, TEM and $163,000 STM/AFM microscopy and BET surface analysis; and DOE Contact: Chet Miller, (202) 586-3952 (3) the extension of in-situ Raman Imaging Naval Research Laboratory Contact: Spectroscopy for conducting remote tests on radioactive David L. Griscom, (202) 404-7087 loaded samples, and for the examination of variations over the surface of large ingots. The research This project is addressing potential hazards of comprises fundamental studies of (1) the relationship radiation-induced gas phase formation in borosilicate between leaching processes and Raman spectroscopy, glasses intended for vitrification of high-level nuclear using both tests on simple liquids and quantum waste. The present research effort is designed to: mechanical modeling; and (2) the examination of (1) demonstrate unambiguously the nature(s) of any transition states in hydration processes involving the radiation-induced gas phases which may be dissolved higher valence and multivalent ions and their use in in high-level-nuclear-waste-glass forms and lead to predicting, with high accuracy, their solubility in bubble formation; (2) provide fundamental knowledge aqueous solutions using both experimental and necessary to assess the vulnerability of these forms to quantum mechanical modeling methods. The chemical explosion, particularly if dissolved oxygen is combination of these two studies has the potential to verified; and (3) develop an efficient method of offer a novel method which has both in-situ and remote surveying wide ranges of potential waste glass capabilities for the analysis of leaching processes on compositions to determine the dependence of radiolytic high-level radioactive waste glasses. This method oxygen evolution on glass composition and hence makes possible tests on radioactive materials with determine compositions with superior resistance to greatly reduced personnel exposure, and makes decomposition. possible the examination of leaching processes in real-time in burial sites. Finally, this method can be Keywords: Borosilicate Glass, Gas Phases, High applied to the continuous monitoring of the conditions of Level Waste glass boules during actual disposal conditions.

Keywords: High Level Waste, Leaching, Glass

143 Office of Environmental Management

305. INVESTIGATION OF MICROSCOPIC practical information, through the conduct of a RADIATION DAMAGE IN WASTE FORMS systematic research activity that utilizes the unique USING ODNMR AND AEM TECHNIQUES facilities at Argonne National Laboratory, e.g., the $232,667 Advanced Photon Source (APS) for X-ray absorption DOE Contact: Chet Miller, (202) 586-3952 spectroscopy (XAS), as well as specialized laboratory Argonne National Laboratory Contact: facilities and instrumentation for carrying out Guokui Liu, (630) 252-4630 experiments with radioactive materials. Formal collaboration with a university assures that a strong This project investigates the microscopic effects of basic approach is taken in the analyses and radiation damage in crystalline and glass high level methodologies used to achieve the desired goals. waste forms (HLW). Information about the nature of electronic interaction and the chemical bonding The research consists of electrochemical studies of the properties of radionuclides in damaged phases is being corrosion and passivation behavior of iron, nickel, developed. Connections between the consequences of chromium, and stainless steel over a wide pH range and alpha and beta-decay processes and radionuclide as a function of temperature from 25 to 95°C. The release and chemical decomposition in waste forms are energetics and dynamics of film formation and being established. Detailed studies focus on the dissolution and the effect of incorporation of heavy microscopic effects of alpha-decay of the transuranic metal ions and radioactive elements are being isotopes 2323pu, 24124Am, and 243244Cm and the beta- investigated. Synchrotron X-ray absorption and and alpha-decay of 249Bk(249Cf) doped into crystalline vibrational (infrared and Raman) spectroscopic materials 10 to 30 years ago and currently prepared techniques are being used to define in-situ the structure borosilicate glasses. Electronic and chemical binding and composition of the various oxide phases that are properties and local structural changes of parent formed as a function of temperature. radionuclide species and their decay daughters in the radiation damaged regions of the waste forms are being Keywords: Surface Films, Metals, Piping, Waste probed using nonlinear laser spectroscopic techniques, Tanks such as optically detected nuclear magnetic resonance (ODNMR), in concert with analytical electron 307. DETERMINATION OF TRANSMUTATION microscopy (AEM) imaging and analysis and X-ray EFFECTS IN CRYSTALLINE WASTE FORMS diffraction methods. Experimental information obtained $304,328 using various techniques for the same materials is DOE Contact: Chet Miller, (202) 586-3952 being compared and systematic measurements are Argonne National Laboratory Contact: being made after the samples undergo a series of Denis M. Strachan, (630) 252-4479 annealing tests. Theoretical models based on electronic PNNL Contact: Nancy J. Hess, and nuclear interactions of the actinides and their (509) 375-2142 surrounding ligands are being developed to interpret the experimental results and correlate the microscopic The objective of this study is to characterize the effects effects of radiation damage to the macroscopic of transmutation in a candidate waste form for ' 37Cs by mechanical and chemical properties of the HLW investigating samples of a cesium aluminosilicate materials. mineral, pollucite, that have undergone "natural" decay of the Cs under ambient temperature while isolated Keywords: High Level Waste, Radiation Damage from interfering chemical effects. There currently is no information on P-decay transmutation effects in waste 306. IN-SITU SPECTRO-ELECTROCHEMICAL forms in which transmutation has occurred over the STUDIES OF RADIONUCLIDE CONTAMINATED natural decay time of the decaying isotope. This causes SURFACE FILMS ON METALS AND THE large uncertainty as to the effect of the transmutation on MECHANISM OF THEIR FORMATION AND the physical and chemical properties of the waste form. DISSOLUTION As a result, uncertainties arise about the viability of the $335,000 waste form as a long-term storage media for nuclear DOE Contact: Chet Miller, (202) 586-3952 waste. Information on the effects of transmutation from Argonne National Laboratory Contact: a-decay will give support to the selection of alternate Carlos A. Melendres, (630) 252-4346, waste forms for separated 137Cs and give information on Northern Illinois University Contact: the long-term behavior of candidate waste forms. S. M. Mini, (815) 753-6484 The approach is to nondestructively examine small The aim of this research is to gain a fundamental stainless steel capsules containing pure pollucite. The understanding of the structure, composition, and contents of these capsules will be examined with mechanism of formation of radionuclide-containing XANES, XAFS, and small angle anomalous X-rays. The surface films on metals that are relevant to the problem synchrotron facilities at Stanford and ANL will be of decontamination of piping systems and waste storage tanks at DOE nuclear facilities. This project seeks to expand our knowledge, while obtaining useful

144 Office of Environmental Management utilized. The scientific team is comprised of members nuclear weapons production facilities. Such additional from PNNL, ANL, and LANL. costs may be avoided by developing a small number of alternative waste glasses which are suitable for vitrifying Keywords: Transmutation, Crystalline Waste Forms, those specific waste feeds that are incompatible with Synchrotron Radiation Facilities borosilicate glasses.

308. RADIATION EFFECTS ON MATERIALS IN THE An alternative waste form based on a new family of NEAR-FIELD OF NUCLEAR WASTE iron-phosphate glasses which appear to be well suited REPOSITORY for many waste feeds, especially those which are $136,000 incompatible with borosilicate glasses, has recently DOE Contact: Chet Miller, (202) 586-3952 been developed. University of Michigan Contacts: Lu-Min Wang, (313) 647-8530 and More information on the atomic structure, valence Rodney C. Ewing, (313) 647-8529 states, nature of bonding, structure-property relationships, crystallization kinetics, and optimized melt Successful, demonstrated containment of radionuclides processing conditions is needed for iron phosphate in the near-field can greatly reduce the complexity of the glasses and their waste forms. This research is using performance assessment analysis of a geologic techniques such as EXAFS, XANES, XPS, X-ray and repository. The chemical durability of the waste form, neutron diffraction, IR, SEM, Mossbauer spectroscopy the corrosion rate of the canister, and the physical and and DTA/DSC to obtain the information needed to chemical integrity of the back-fill provide important demonstrate that iron phosphate waste forms can meet barriers to the release of radionuclides. However, the stringent requirements for nuclear waste disposal. near-field containment of radionuclides depends critically on the behavior of these materials in a Keywords: Iron Phosphate Glasses, Vitrification, radiation field. Nuclear Waste A systematic study is being performed of elastic and 310. MICROSTRUCTURAL PROPERTIES OF HIGH inelastic damage effects in materials in the near-field. LEVEL WASTE CONCENTRATES AND GELS These include: (1) waste forms (glass and crystalline WITH RAMAN AND INFRARED ceramics); (2) alteration products of waste forms (clays SPECTROSCOPIES and zeolites); (3) back-fill materials (clays and zeolites). $155,000 The work draws on over twenty years of experience in DOE Contact: Chet Miller, (202) 586-3952 studying radiation effects in minerals and complex Los Alamos National Laboratory Contact: ceramics and utilizes an unusual combination of studies Stephen F. Agnew, (505) 665-1764 of natural phases of great age with ion beam and electron irradiations of synthetic phases under carefully Nearly half of the high level radioactive waste stored at controlled conditions. Hanford is composed of highly alkaline concentrates referred to as either salt cakes or Double-Shell Slurry Keywords: Radiation Effects, Near-field, Geologic (DSS), depending on their compositions and processing Repository histories. The major components of these concentrates are water, sodium hydroxide, and sodium salts of 309. AN ALTERNATIVE HOST MATRIX BASED ON nitrate, nitrite, aluminate, carbonate, phosphate, and IRON PHOSPHATE GLASSES FOR THE sulfate. In addition, there are varying amounts of VITRIFICATION OF SPECIALIZED NUCLEAR assorted organic salts such as EDTA, glycolate, and WASTE FORMS citrate. Although measurements of the bulk properties of $208,278 these wastes, such as viscosity, gel point, density, etc., DOE Contact: Chet Miller, (202) 586-3952 have been exhaustively reported in the past, little is University of Missouri-Rolla Contact: known about how those macroscopic characteristics are Delbert E. Day, (573) 341-4354 related to the microscopic physical and chemical properties of the waste. Such characteristics as Borosilicate glass is the only material currently viscosity, solids volume percent, and gas retention can approved and being used to vitrify high level nuclear change dramatically with relatively small changes in waste. Unfortunately, many high level nuclear waste composition and temperature and these same feeds in the U.S. contain components which are properties are important for the determination of safe chemically incompatible with borosilicate glasses. storage conditions as well as in planning retrieval, Current plans call for vitrifying even these problematic pretreatment, and disposal of the wastes. waste feeds in borosilicate glasses after the original waste feed has been pre-processed and/or diluted to The aim of this work is to use FTIR, Raman, and NMR compensate for the incompatibility. However, these spectroscopies, along with thermophysical heats of pre-treatment processes, as well as the larger waste gelation, to relate the microstructural, physical and volumes resulting from dilution. will add billions of chemical properties of these concentrates to their dollars to the DOE's cost of cleaning up the former macroscopic characteristics. With this better

145 Office of Environmental Management

understanding of macroscopic characteristics, the DOE substituted zirconolite and pyrochlore, and develop an will be in a better position to safely store these wastes understanding of the bonding characteristics and as well as to be able to better plan for their retrieval, stabilities of these materials. pretreatment, and final disposal. These microscopic properties are being related to the macroscopic Keywords: High Temperature Solution Calorimetry, characteristics by using: Actinides

* Water vapor pressure measurements for 312. PHOTOOXIDATION OF ORGANIC WASTES concentrates to unambiguously determine water USING SEMICONDUCTOR NANOCLUSTERS activity as a function of composition and $417,000 temperature. DOE Contact: Chet Miller, (202) 586-3952 SNL Contact: J. P. Wilcoxon, (505) 844-3939 * FTIR, Raman, and Al NMR spectroscopies to Colorado State University Contact: D. F. Kelley, determine the form and solubility of aluminate in (970) 491-6381 caustic slurries. Solar detoxification is a process wherein sunlight is * Micro-Raman spectroscopy to identify and quantify captured by a semiconductor particle in suspension to phases of each species for a variety of concentrates. create electrons and holes that then diffuse to the particulate surface to effect the oxidation and reduction * Measurements of the heat of gelation and its of toxic pollutants. Using solar energy to oxidize organic dependence on water activity, presence of organic, chemicals to carbon dioxide and dilute mineral acids is and other properties. very energy efficient compared to other methods such as incineration. Finding an efficient particulate has thus Keywords: High Level Waste, Raman Spectroscopy, been a focus of research, which has had only limited Infrared Spectroscopy success, the fundamental problem being that materials that efficiently absorb in the visible portion of the solar 311. FUNDAMENTAL THERMODYNAMICS OF spectrum also photocorrode. ACTINIDE-BEARING MINERAL WASTE FORMS $383,333 Past solar detoxification efforts have relied almost DOE Contact: Chet Miller, (202) 586-3952 exclusively on titanium dioxide, and although it is Los Alamos National Laboratory Contact: photostable, it is a white material with a UV bandgap Mark A Williamson, (505) 667-4045 that absorbs less than 7% of the solar spectrum. It also LLNL Contact: Bartley B. Ebbinghaus, suffers from electron-hole recombination in commer- (510) 422-8792 cially available forms. Recent research has made UC Davis Contact: Alexandra Navrotsky, possible the synthesis of photostable semiconductor (916) 752-3292 nanoclusters with visible band gaps that can be tuned by adjusting the cluster size. Thus bulk materials with The end of the Cold War raised the need for the near IR absorbence edges can be made into visible technical community to be concerned with the band-edge materials with stronger redox potentials. disposition of excess nuclear weapon material. The plutonium will either be converted into mixed-oxide fuel The rate of electron-hole recombination is small in for use in nuclear reactors or immobilized in glass or nanoclusters, so they have the potential to act as highly ceramic waste forms and placed in a repository. The efficient solar detoxification agents. In effect, they act stability and behavior of plutonium in the ceramic more like molecular organic photoredox catalysts, but materials as well as the phase behavior and stability of with significant advantages in chemical stability the ceramic material in the environment is not well because they are inorganic. This project is investigating established. In order to provide technically sound the use of these materials in practical detoxification solutions to these issues, thermodynamic data are applications. essential in developing an understanding of the chemistry and phase equilibria of the actinide-bearing Keywords: Photooxidation, Nanoclusters mineral waste form materials proposed as immobilization matrices. Mineral materials of interest include zircon, zirconolite, and pyrochlore. High temperature solution calorimetry is one of the most powerful techniques, sometimes the only technique, for providing the fundamental thermodynamic data needed to establish optimum material fabrication parameters, and, more importantly, to understand and predict the behavior of the mineral materials in the environment. The purpose of this project is to experimentally determine the enthalpy of formation of actinide orthosilicates, the enthalpies of formation of actinide

146 Office of Environmental Management

313. OPTIMIZATION OF THERMOCHEMICAL, laboratory tests. The role of nitrite has not been KINETIC, AND ELECTROCHEMICAL FACTORS explained electrochemically in a general manner that GOVERNING PARTITIONING OF permits the prediction of nitrite effectiveness in solutions RADIONUCLIDES DURING MELT of widely varied composition. DECONTAMINATION OF RADIOACTIVELY CONTAMINATED STAINLESS STEEL A model is being developed of the nitrite concentration $400,000 required to prevent pitting corrosion in terms of the DOE Contact: Chet Miller, (202) 586-3952 electrochemical and surface oxide properties of the SNL Contact: James A. Van den Avyle, carbon steel solution system for a wide range of (505) 845-3105 solution compositions. Typical industrial salt solutions contain numerous ionic species and suspended Melt Decontamination represents an effective scrap insoluble compounds, as well as dissolved organic metal recycling route for the estimated 1,200,000 tons species. of contaminated stainless steel and nickel currently within the DOE complex. At present, this material must Keywords: Pitting Corrosion, Nitrite, Carbon Steel be considered a substantial disposal liability. However, with appropriate recycling, this material may be 315. STABILITY OF HIGH-LEVEL WASTE FORMS regarded as an asset worth an estimated $5 billion. The $254,000 goal of this project is to optimize a melt decontami- DOE Contact: Chet Miller, (202) 586-3952 nation process through a basic understanding of the Oak Ridge National Laboratory Contact: factors which govern the partitioning of various Theodore M. Besmann, (423) 574-6852 radionuclides between the metal, slag, and gas phases. Radionuclides which are captured by a slag phase may The assessment of release of radionuclides from waste be stabilized by promoting the formation of synthetic repositories depends substantially on the leaching minerals within a leach-resistant matrix. This research behavior of the spent fuel or waste form. Assumed rates describes an integrated program of simulation and based on dissolution of specific phases (assumption of experimentation designed to investigate and optimize unit activity) will lead to potentially grossly overesti- liquid metal techniques for the decontamination and mated values as well as possibly underestimated recycling of radioactive scrap metal. values, and are therefore difficult to defend. Current, experimentally-determined values are less than Keywords: Melt Decontamination, Radioactive Scrap desirable since they depend on measurement of the Metal leach rate under non-realistic conditions designed to accelerate processes that are geologic in time scale. 314. MECHANISM OF PITTING CORROSION With the possible consideration of a hot repository for PREVENTION BY NITRITE IN CARBON STEEL the disposal of spent fuel and high-level waste forms, EXPOSED TO DILUTE SALT SOLUTIONS the materials will experience elevated temperatures (> $216,667 100°C) for hundreds of years or longer, driving DOE Contact: Chet Miller, (202) 586-3952 chemical and phase changes. The objective of the effort Savannah River Technology Center is to develop a basic understanding of the phase Contact: Philip E. Zapp, (803) 725-2567 equilibria and solid solution behavior of the constituents University of South Carolina Contact: of high-level waste forms and to model that behavior. John Van Zee, (803) 777-2285 The results of this effort will provide reaction path information for leaching/transport codes such as ESP, The overall goal of this project is to develop a as well as basic insights into complex ceramic solution fundamental understanding of the role of nitrite in behavior, bonding in glasses, and crystal chemistry of preventing the breakdown of protective oxide coating on the fluorite-structure uranium dioxide-fission product steel and the onset of pitting. A fundamental system. understanding of the materials science and electrochemistry of the nitrite role is expected to lead to Keywords: Spent Fuel, High Level Waste, Leaching, superior and more cost-effective corrosion prevention Transport methods for storing and processing complex, industrially important salt solutions. One important application of this new information in the DOE complex involves the high-level radioactive waste solutions contained in carbon steel tanks.

There is an extensive base of engineering knowledge of corrosion prevention by nitrite in alkaline salt solutions containing various organic and inorganic aggressive species. This knowledge is empirical; effective nitrite concentrations have been related to solution composition and temperature through numerous

147 Office of Environmental Management

316. RADIATION EFFECTS IN NUCLEAR WASTE at Pacific Northwest National Laboratory that shows MATERIALS that thermally treated CSTs have durabilities better than $960,000 borosilicate glass. The goal of the program is to reduce DOE Contact: Chet Miller, (202) 586-3952 the costs associated with CST waste disposal, to PNNL Contact: William J. Weber, minimize the risk of contamination to the environment (509) 375-2299 during CST processing, and to provide DOE with Argonne National Laboratory Contact: technical alternatives for CST disposal. Because there R. B. Bircher, (630) 252-4996 is uncertainty in repository availability and in waste LANL Contact: Michael A. Nastasi, acceptance criteria, it is likely that Cs and Sr loaded ion (505) 667-7007 exchangers will require short term storage at Hanford or University of Michigan Contact: that new scenarios for long term storage or disposal of Rodney C. Ewing, (313) 647-8529 nuclides with relatively short half lives (such as ' 37Cs and 90Sr) will arise. The objective of this multidisciplinary, multi-institutional research effort is to develop a fundamental under- This research synthetically explores both low and high standing at the atomic, microscopic, and macroscopic temperature stable and metastable phases involving the levels of radiation effects in glass and ceramics that key component elements. This allows for characteri- provides the underpinning science and models for zation of all potential by-products from thermal evaluation and performance assessments of glass and treatment of CSTs. The technical objective of the work ceramic waste forms for the immobilization and is to (1) fully characterize the phase relationships, disposal of high-level tank waste, plutonium residues structures and thermodynamic and kinetic stabilities of and scrap, surplus weapons plutonium, and other crystalline silocotitanate waste forms, and (2) to actinides. Studies focus on the effects of ionization and establish a sound technical basis for understanding key elastic-collision interactions on defect production, defect waste form properties, such as melting temperatures interactions, structural rearrangements, diffusion, and aqueous durability, based on an in-depth under- solid-state phase transformations, and gas standing of waste form structures and thermochemistry. accumulation using actinide containing materials, gamma irradiation, ion-beam irradiation and Keywords: Silicotitanate, Waste Form electron-beam irradiation to simulate the effects of alpha decay and beta decay on nuclear waste glasses 318. ION-EXCHANGE PROCESSES AND and ceramics. This program exploits a variety of MECHANISMS IN GLASSES structural, optical, and spectroscopic probes to $300,333 characterize the nature and behavior of the defects, DOE Contact: Chet Miller, (202) 586-3952 defect aggregates, and phase transformations. PNL Contact: B. Peter McGrail, Computer simulation techniques are used to determine (509) 376-9193 defect production from ballistic and ionization LBNL Contact: David K. Shuh, interactions, calculate defect stability, energies of (510) 486-6937 formation and migration, damage processes within an alpha-recoil cascade, and defect/gas diffusion and Recent performance assessment calculations of a interaction. disposal system at Hanford, Washington for low activity waste glass show that a Na ion-exchange reaction can Keywords: Glass, Ceramics, Radiation Effects effectively increase the radionuclide release rate by over a factor of 1000 and so is a major factor that currently 317. NEW SILICOTITANATE WASTE FORMS: limits waste loading. However, low temperature ion DEVELOPMENT AND CHARACTERIZATION exchange has not been thought to be important in $400,000 recent analyses of waste glass durability. The objective DOE Contact: Chet Miller, (202) 586-3952 of this work is to develop an understanding of the PNL Contact: Mar Lou Balmer, processes and mechanisms controlling alkali ion (509) 372-4693 exchange and to correlate the kinetics of the SNL Contact: Tina Nenoff, (505) 844-0340 ion-exchange reaction with glass structural properties. UC Davis Contact: Alexandra Navrotsky, (916) 752-3292 Ion-exchange reaction mechanisms are being studied by using nuclear reaction analysis techniques to probe This program outlines a new strategy for disposing of the distribution of isotopically-labeled elements in the crystalline silicotitanate (CST) ion exchangers by in situ hydrated layers on glass surfaces. Differences in the heat treatment to produce an alternate waste form. New uptake and distribution of these isotopes provide a waste forms and disposal strategies specific to CST signature characteristic of specific ion-exchange secondary waste that are developed in this work will reactions. X-ray absorption spectroscopy is used to offer an alternative to current disposal plans which call identify and correlate key structural properties, such as for recombining the separated Cs, Sr-loaded CST into the number of nonbridging oxygens, bonding of alkali to the high activity waste streams then dissolving it in other elements in the glass, and alkali coordination, with borosilicate glass. This research is predicated by work differences in measured rates of alkali exchange. The

148 Office of Environmental Management fundamental understanding of the ion-exchange process 320. MODELING OF DIFFUSION OF PLUTONIUM IN developed under this study will provide a sound OTHER METALS AND OF GASEOUS SPECIES scientific basis for formulating low exchange rate IN PLUTONIUM-BASED SYSTEMS glasses with higher waste loading, resulting in $145,000 substantial production and disposal cost savings. DOE Contact: Chet Miller, (202) 586-3952 West Virginia University Contact: Keywords: Ion-exchange, Glasses Bernard R. Cooper, (304) 293-3423 University of Connecticut Contact: 319. DISTRIBUTION & SOLUBILITY OF RADIO- Gayanath Fernando, (860) 486-0442 NUCLIDES & NEUTRON ABSORBERS IN WASTE FORMS FOR DISPOSITION OF The research is aimed at developing and utilizing PLUTONIUM ASH & SCRAPS, EXCESS computational-modeling-based methodology to treat PLUTONIUM, AND MISCELLANEOUS SPENT two major problems. The first of these is to be able to NUCLEAR FUELS predict the diffusion of plutonium from the surface into $600,000 the interior of another metal such as uranium or DOE Contact: Chet Miller, (202) 586-3952 stainless steel (fcc iron). The second is the more PNNL Contact: Xiangdong Feng, complicated situation of treating the diffusion of a (509) 373-7284 gaseous species into plutonium-containing oxidized Australian Nuclear Science & Technology material, specifically the solid-state diffusion of Organisation Contact: Eric R. Vance O2-driven by an oxygen gradient. The first class of LBNL Contact: David K. Shuh, (510) 486-6937 problem, diffusion of plutonium into host metals, is University of Michigan Contact: pertinent to characterizing contamination and Rodney C. Ewing, (313) 647-8529 consequent clean-up procedures in situations where plutonium has been in contact with other metals for The objective of this multi-institutional, multi-national extended periods of time. The second situation is research effort is to understand the distributions, pertinent to complicated hydrogen generation solubilities, and releases of radionuclides and neutron mechanisms creating possibly catastrophic pressure in absorbers in waste forms. The results will provide the situations, such as storage barrels, where oxidized underpinning knowledge for developing, evaluating, plutonium-containing material has been stored for long selecting, and matching waste forms for the safe periods of time. disposal of various wastes associated with Pu, miscellaneous spent nuclear fuels (SNF), and other The investigation of thermally-activated diffusion makes transuranic (TRU) wastes and for developing use of transition state theory with dynamic corrections. deterministic model for the long-term performance In transition state theory the number of crossings of a assessment of radionuclide containment. specified counting surface that separates initial and final states is equated to the number of such crossings that The scope of this project includes: (1) systematically occur in an equilibrium system. The use of ab-initio- investigate the solubility and partition behavior of based atomistic potentials allows efficient mapping of selected waste forms as a function of composition, the pertinent energy barriers. Molecular dynamics can temperature, and processing conditions with the goal of be used to treat realistically the nature of the hoppings enhancing our understanding of the physics and as well as to correct for dynamical effects such as chemistry of radionuclides and neutron absorbers in recrossings. Grain boundaries are simulated and simplified waste forms; (2) determine the local structure incorporated into dynamic simulations to study the of radionuclides and neutron absorbers waste forms in relative importance of grain boundary diffusion in various phases: (a) develop a microscale characteri- allowing plutonium atoms to penetrate into the interior zation to determine what phases are presented and how of the host metals. key elements are partitioned among those phases using optical, scanning, and transmission microscopies and The two main components of the modeling study are: XRD; (b) develop a molecular level characterization to (1) the treatment of diffusion and of the pertinent grain understand local coordination using EXAFS and NMR; boundary modeling and (2) the development of (c) an atomic level characterization to determine physically accurate plutonium atomistic potentials. The oxidation state using XANES; (3) selectively study physical quality of these potentials is the controlling waste form properties with the emphasis on the release quantity in determining the ability to be accurately behaviors of neutron absorbers and radionuclides. predictive for the questions of interest. Keywords: Radionuclides, Neutron Absorbers, Keywords: Diffusion, Plutonium, Modeling and Solubility, Waste Form Simulations

149 Office of Nuclear Energy, Science and Technology

OFFICE OF NUCLEAR ENERGY, SCIENCE AND TECHNOLOGY FY 1997

Office of Nuclear Enerav. Science and Technoloav - Grand Total $65,080,000

Office of Engineering and Technologa Development $ 2,080,000

Space and National Security Proarams $ 2,080,000

Materials Preparation. Synthesis. Deposition. Growth or Forming $ 1,815,000 Development of an Improved Process for the Manufacture of DOP-26 Iridium Alloy Blanks, Product Characterization and Exploratory Alloy Improvement Studies 1,425,000 Carbon-Bonded Carbon Fiber Insulation Production Maintenance, Manufacturing Process Development and Product Characterization 390,000 Materials Properties. Behavior. Characterization or Testing $ 265,000

Development of Materials for Advanced Radioisotope Power Systems 265,000

Office of Naval Reactors $63,000,0001

'This excludes $47 million for the cost of irradiation testing in the Advanced Test Reactor (ATR).

150 Office of Nuclear Energy, Science and Technology

OFFICE OF NUCLEAR ENERGY, SCIENCE AND TECHNOLOGY

OFFICE OF ENGINEERING AND TECHNOLOGY Iridium process improvement activities were continued. DEVELOPMENT Bare rolling is ready for introduction into the sheet production process. Bare cup forming development was SPACE AND NATIONAL SECURITY PROGRAMS continued. Scale-up and evaluation of a new DOP-40 low thorium alloy (lr-0.3 wt. % tungsten with dopant Space and National Security Programs include the additions of 40 ppm cerium and 15 ppm thorium) was development and production of radioisotope power continued. systems for both space and terrestrial applications and the technical direction, planning, demonstration and Keywords: Consumable Arc Melt, Extrusion, Noble delivery of space nuclear reactor power and propulsion Metal, Rolling, Forming systems. During FY 1997, space nuclear reactor power and propulsion activities remained dormant. Essentially 322. CARBON-BONDED CARBON FIBER all materials programs were aimed at: (1) support of INSULATION PRODUCTION MAINTENANCE, the production of General Purpose Heat Source- MANUFACTURING PROCESS DEVELOPMENT Radioisotope Thermoelectric Generators for the NASA AND PRODUCT CHARACTERIZATION Cassini Mission, (2) maintenance of iridium alloy and $390,000 carbon bonded carbon fiber insulation heat source DOE Contact: W. Barnett, (301) 903-3097 components manufacturing capability, (3) continued ORNL Contacts: R. Dinwiddie, (615) 574-9978 improvement in heat source materials and their and D. J. McGuire, (423) 574-4835 production processes and product characterization, and (4) materials (non-thermoelectric) support for future Carbon-bonded carbon fiber (CBCF) type thermal high efficiency advanced radioisotope power systems. insulation material is employed in Isotopic General Purpose Heat Source (GPHS) Module assemblies for MATERIALS PREPARATION, SYNTHESIS, use in current GPHS-RTG (radioisotope thermoelectric DEPOSITION, GROWTH OR FORMING generator). This material was originally employed in GPHS-R7Gs for the Galileo/NASA (1989 launch) and 321. DEVELOPMENT OF AN IMPROVED PROCESS Ulysses/NASA-ESA (1990 launch) Missions. Material FOR THE MANUFACTURE OF DOP-26 IRIDIUM produced for the Cassini Mission (1997 launch) was ALLOY BLANKS, PRODUCT CHARACTERIZA- made with a replacement carbon fiber (new vendor, TION AND EXPLORATORY ALLOY former source not available) utilizing an optimized IMPROVEMENT STUDIES process and process controls. The FY 1997 program $1,425,000 encompassed (1) continued maintenance of capability DOE Contact: W. Barnett, (301) 903-3097 for both tube and plate billet production, (2) continued ORNL Contacts: E. P George, characterization of Cassini CBCF insulation high (615) 574-5085 and E. K. Ohriner, temperature thermal conductivity, and (3) study of the (615), 574-8519 role of inert additives on high temperature thermal conductivity. An iridium alloy, DOP-26 (i.e., lr-0.3 wt.% W with Th and Al dopant additions), serves as the fuel clad or Keywords: Insulators/Thermal, High Temperature capsule material for isotope heat sources employed in Service, Fibers recent and contemporary space power systems for NASA deep space missions. This program is aimed at MATERIALS PROPERTIES, BEHAVIOR, the optimization of the new improved process route CHARACTERIZATION OR TESTING previously selected for the production of DOP-26 iridium alloy sheet, namely a consumable vacuum arc cast/ 323. DEVELOPMENT OF MATERIALS FOR extrusion/warm' rolling route. The effectiveness of this ADVANCED RADIOISOTOPE POWER production process was further demonstrated in the SYSTEMS production of DOP-26 alloy blanks, foil and clad vent $265,000 sets for the Cassini Mission. Production yields have DOE Contact: W. Barnett, (301) 903-3097 continued to exceed our goals. Oak Ridge National Laboratory Contact: J. King, (423) 574-4807 During FY 1997, production of DOP-26 iridium alloy blanks, foil and clad vent set hardware for the Cassini Materials support was provided for two advanced mission was completed. Transfer of the clad vent set radioisotope power systems, namely a heat source for a manufacturing operation from the Y-12 plant to the Oak small Stirling Engine and an Alkali metal Thermal to Ridge National Laboratory was initiated. Iridium alloy Electric Converter (AMTEC) Cell. manufacturing capabilities are being maintained in a production maintenance mode.

151 Office of Nuclear Energy, Science and Technology

Long-term intermediate temperature creep properties of T-111 tantalum alloy were continued. Evaluation of the high temperature reflectivity of rhodium plated Haynes-25 alloy was initiated.

Keywords: Tantalum Alloy, Creep, Rhodium Plate, Reflectivity

OFFICE OF NAVAL REACTORS

The materials program supports the development and operation of improved and longer life reactors and pressurized water reactor plants for naval nuclear propulsion.

The objective of the materials program is to develop and apply, in operating service, materials capable of use under the high power density and long life conditions required of naval ship propulsion systems. This work includes irradiation testing of reactor fuel, poison, and cladding materials in the Advanced Test Reactor at the Idaho National Engineering Laboratory. This testing and associated examination and design analysis demonstrates the performance characteristics of existing materials as well as defining the operating limits for new materials. Corrosion, mechanical property, and wear testing is also conducted on reactor plant structural materials under both primary reactor and secondary steam plant conditions to confirm the.acceptability of these materials for the ship life. This testing is conducted primarily at two Government laboratories-Bettis Atomic Power Laboratory in Pittsburgh and Knolls Atomic Power Laboratory in Schenectady, New York. One result of the work on reactor plant structural material is the issuance of specifications defining the processing and final product requirements for materials used in naval propulsion plants. These specifications also cover the areas of welding and nondestructive testing.

Funding for this materials program is incorporated in naval projects jointly funded by the Department of Defense and the Department of Energy. This funding amounts to approximately $110 million in FY1997 including approximately $47 million as the cost for irradiation testing in the Advanced Test Reactor. The Naval Reactors contact is David I. Curtis, (703) 603-5565.

152 Office of Civilian Radioactive Waste Management

OFFICE OF CIVILIAN RADIOACTIVE WASTE MANAGEMENT

FY 1997

Office of Civilian Radioactive Waste Manaaement - Grand Total $15,400,000 Materials Properties. Behavior. Characterization or Testing $15,400,000

Waste Packages $15,400,000

153 Office of Civilian Radioactive Waste Management

OFFICE OF CIVILIAN RADIOACTIVE WASTE MANAGEMENT

Materials research is ongoing in the Office of Civilian Radioactive Waste Management in the development of waste packages for eventual geologic disposal.

MATERIALS PROPERTIES, BEHAVIOR, canistered SNF, canistered defense high-level waste, CHARACTERIZATION OF TESTING Navy fuel, and other DOE owned spent nuclear fuel. The analytical process that is underway to support 324. WASTE PACKAGES these designs included thermal, structural, and $15,400,00 neutronic analyses. Also included are materials DOE Contact: David Haught, (702) 794-5474 selection and engineering development. The waste M&O Contacts: Hugh Benton, package materials effort includes the testing and (702) 295-4389 and David Stahl, modeling of materials being considered for inclusion in (702) 295-4383 the waste package and the engineered barrier system. The testing includes general aqueous and atmospheric The development of the nation's high-level waste testing, localized attack such as pitting and service repository has been delegated to DOE's Yucca corrosion, microbiologically-influenced corrosion, Mountain Site Charactization Project Office. Framatome galvanic corrosion, and stress corrosion cracking. The Cogema Fuels (formerly B&W Fuel Company), as part corrosion test facility started the long-term (at least five- of the Civilian Radioactive Waste Management System year) test program in FY 1996 with corrosion-allowance Management & Operating (M&O) Contractor, is materials. Corrosion-resistant materials were added in responsible for designing the waste package and related FY 1997. Waste form materials are also being portions of the engineered barrier system. The evaluated for alteration and leaching under repository- advanced conceptual design was completed in 1996. relevant conditions. Chemical simulations have been Progress on the waste package and the supporting performed to evaluate the performance of engineered materials studies has been documented in various barrier materials. These latter efforts support both reports. design and performance assessment. The waste package design effort includes the Keywords: Yucca Mountain Repository, Waste development of waste packages to accommodate Package, Engineered Barrier System uncanistered commercial spent nuclear fuel (SNF),

154 Office of Fossil Energy

OFFICE OF DEFENSE PROGRAMS FY 1997

Ofice of Defense Programs - Grand Total $96,633,600 The Weapons Research. Development and Test Program $96,633,600

Sandia National Laboratories $23,183,600

Materials Preparation. Synthesis. Deposition. Growth or Forming $ 6,231,000

Materials Processing 2,999,000 Sol-Gel Preservation of Mankind's Cultural 137,000 Synthesis and Modeling of Field-Structured Anisotropic Composites 370,000 Molecular Imprinting in Aerogels for Remote Sensing of Chemical Weapons and Pesticides 390,000 Smart Interface Bonding Alloys (SIBA): Tailoring Thin Film Mechanical Properties 455,000 Atomically-Engineered Nanostructures: An Interdisciplinary Approach Properties 400,000 Enabling Science & Technology for Cold Spray Direct Fabrication Properties 330,000 Atomic-Level Studies of Surfactant-Directed Materials Growth 400,000 Freeforming of Ceramics and Composites from Colloidal Slurries 450,000 Laser Assisted Arc Welding for Aluminum Alloys 200,000 System Studies in Electrochemical Processing Properties 100,000 Materials Properties. Behavior. Characterization or Testing $11,227,000

Aging and Reliability 1,997,000 Nanoscale Structures and Phenomena 1,070,000 Applications-Driven Interdisciplinary Research 885,000 Materials Stability and Thin Coatings 2,483,000 Catalytic Membrane Sensors 361,600 Photonic Band Gap Structures as a Gateway to Nano-Photonics 375,000 Model Determination and Validation for Reactive Wetting Processes 351,000 Ultra-hard Multilayer Coatings Properties 472,000 Molecular-Scale Lubricants for Micromachine Applications 475,000 Understanding and Control of Energy Transfer Mechanisms in Optical Ceramics Properties 400,000 Integrated Thin Film Structures for IR Imaging Properties 430,000 The Initiation and Propagation of Nano-Scale Cracks at an Adhesive/Solid Interface Properties 400,000 Monolithic Structures for Nanoseparation Properties 339,000 Fundamental Aspects of Micromachine Reliability 350,000 Intelligent Polymers for Nanodevice Performance Control 439,000 Quantum Dot Arrays 400,000 Device or Components Fabrication. Behavior or Testing $ 1,522,600

Wide-Bandgap Compound Semiconductors to Enable Novel Semiconductor Devices Project 290,000 Scanning Probe-Based Processes for Nanometer-Scale Device Fabrication 442,600 Surface Micromachined Flexural Plate Wave Device Integrated on Silicon 525,000 Modeling Electrodeposition for Metal Microdevice Fabrication Properties 265,000

Instrumentation and Facilities $ 4,203,000 Advanced Analytical Techniques 998,000 Nanostructures, Advanced Materials and Ion Beam Sciences 2,792,000 Physico-Chemical Stability of Solid Surfaces 413,000

155 Office of Fossil Energy

OFFICE OF DEFENSE PROGRAMS (continued) FY 1997

The Weapons Research. Development and Test Program (continued) Lawrence Livermore National Laboratory $20,250,000

Materials Preparation. Synthesis. Deposition. Growth or Forming $ 7,775,000

Engineered Nanostructure Laminates 2,000,000 Sol Gel Coatings 335,000 KDP and DKDP Crystal Development and Production 4,000,000 Energetic Materials Strategic Chemistry 350,000' CHEETAH Thermochemical Code 190,0001 Explosives Development 900,0001

Materials Properties. Behavior. Characterization or Testing $ 2,250,000

Interfaces, Adhesion, and Bonding 250,000 Laser Damage: Modeling and Characterization 1,000,000 KDP Characterization 1,000,000

Instrumentation and Facilities $10,225,000

Scanning Tunneling Microscopy (STM) and Atomic Force Microscopy (AFM) 250,000 Fatigue of Metal Matrix Composites 500,000 Materials Produced with Dynamic High Pressure 50,000 Properties of Hydrogen at High Shock Pressures and Temperatures 400,000 Atomic Level Explosive Calculations 400,000 Metastable Solid-Phase High Energy Density Materials 535,000 AFM Investigations of Crystal Growth 290,000 Uranium Casting Program 1,000,000 Uranium Spin Forming 1,500,000 Plutonium Near Net Shape Casting 2,500,000 Electron Beam Cold Hearth Melting of Uranium 900,000 NIF Capsule Mandrel R&D 800,000 Polyimide Coating Technology for ICF Targets 500,000 Beryllium Ablator Coatings for NIF Targets 600,000

Los Alamos National Laboratory $53,200,000

Materials Preparation. Synthesis. Deposition. Growth or Forming $ 2,500,000

Rapid Solidification Processing 500,000 Structural Alloy Development 2,000,000 Materials Structure or Composition $ 3,300,000

National High Magnetic Field Laboratory 1,800,000 Neutron Diffraction 1,500,000

'This activity is jointly funded (50:50) by DOE DP and the DoD.

156 Office of Fossil Energy

OFFICE OF DEFENSE PROGRAMS (continued) FY 1997

The Weapons Research. Development and Test Program (continued) Los Alamos National Laboratory (continued)

Materials Properties. Behavior. Characterization or Testing $18,300,000

Dynamic Mechanical Properties of Weapons Materials 2,000,000 Deformation Characterization and Modeling 5,000,000 Materials Aging 11,000,000 Powder Characterization 300,000

Device or Component Fabrication. Behavior or Testing $29,100,000

Manufacturing Process Development 8,000,000 Advanced Engineering Methods Development 1,100,000 Component Fabrication 10,000,000 Laser Target Fabrication 5,000,000 Pulsed Power Target Fabrication 3,000,000 Advanced Strategic Computing Initiative Materials Modeling 2,000,000

157 Office of Fossil Energy

THE WEAPONS RESEARCH, DEVELOPMENT AND infrastructure, environmental contamination by leached TEST PROGRAM mine tailings, protection of ship hulls, and scale formation in petroleum wells.

AH lA LBORATOWEKeywords:NATIONAL Conservation, Sol-Gel 327. SYNTHESIS AND MODELING OF FIELD- MATERIALS PREPARATION, SYNTHESIS, STRUCTURED ANISOTROPIC COMPOSITES DEPOSITION, GROWTH OR FORMING $370,000 DOE Contact: Maurice J. Katz, (202) 586-6385 325. MATERIALS PROCESSING SNL Contact: James Martin, (505) 844-9125 $2,999,000 DOE Contact: Robin Staffin, (202) 586-7590 The modeling, synthesis and processing capability is SNL Contact: John A Sayre, (505) 845-9757 being developed to create novel anisotropic polymer/ ceramic and polymer/metal composite materials by The Materials Processes Program focuses on the applying external electric or magnetic fields to systems research required to create laboratory scale materials consisting of a polymerizable continuous phase into processes for re-manufacturing weapons components which particles having an electric permittivity or by more rapid, predictable, and affordable methods than magnetic permeability mismatch are suspended. A those used in the past. Projects emphasize the linear field will create one-dimensional particle chains, a predictability of microstructure and composition from well known effect. This project used the recent discovery the processing conditions, and the incorporation of this that rotating fields create two-dimensional particle predictability into scientific models and simulations for sheets in the plane of the field. These unique structures use by weapons designers and manufacturing can be captured by polymerizing the continuous phase engineers. A new feature of this thrust is a focus on during a field anneal. A key aspect of this program is processes which enable fabrication with fewer steps modeling and controlling the evolution of structure in from design to product, with the ultimate goal of one-these materials. step fabrication of complex shape parts composed of , , , multiple materials directly from a CAD file.Keywords: Polymer, Ceramic, Metal, Composite Keywords: Processing, Fabrication 328. MOLECULAR IMPRINTING IN AEROGELS FOR REMOTE SENSING OF CHEMICAL WEAPONS 326. SOL-GEL PRESERVATION OF MANKIND'S AND PESTICIDES CULTURAL $390,000 $137,000 DOE Contact: Maurice J. Katz, (202) 586-6385 DOE Contact: Maurice J. Katz, (202) 586-6385 SNL Contact: Roger Lee Clough (505) 844-3492 SNL Contact: William Hammetter, (505) 272-7603 Recent events in Japan, Iraq, and elsewhere have underlined the need for reliable, inexpensive sensors for Our cultural heritage, as reflected in artifacts and works chemical warfare agents. Warfare agents, such as of art, is being lost at an astonishing rate due to the sarin, belong to a general class of phosphate and ravages of nature and especially mankind. Since the phosphonate esters that have a very broad range of industrial revolution, chemical by-products of man's activities including materials for nuclear weapons technological advances have caused the deterioration of production, pesticides, genetic material, and biological our most precious cultural treasures. Most vulnerable cellular signals. Current methods to detect these agents are stone objects that are subjected to outdoor are limited to laboratory analysis. An in-field, real-time environments in industrialized or urban settings. This sensor-based approach with remote sensing capability research comprises three basic elements: (1) molecular is highly desired. modeling of the weathering mechanisms and resultant surface structure of model limestones, (2) mineral- Under this project, highly sensitive and specific optical specific passivation of the weathered surface to prevent sensors for phosphate and phosphonate esters are further hydrolytic attack, and (3) in situ polymerization being designed and developed using molecular (within the weathered surface) to form a UV stable recognition sites in high surface area aerogels. network that imparts strength and hydrophobicity. This Molecular recognition sites are engineered using research has been conducted in collaboration with The computer aided molecular design and generated via the Metropolitan Museum of Art (MMA) and The Getty powerful 'template imprinting' technique in aerogels. Conservation Institute (GCI), who have provided The material is designed with active fluorophores at the samples and ensured relevance to the conservation receptor site reporting on target molecule recognition communities. In addition to solving the urgent need to via fluorescence signal through complexation with the preserve our cultural treasures, the methodology phosphonate guest. From these materials are developed here can be applied to other mineral- developed various toxic gas sensor motifs, such as corrosion problems such as the degradation of concrete visual detectors that monitor color changes, or

158 Office of Fossil Energy extremely low level sensing applications that follow 330. ATOMICALLY-ENGINEERED fluorescence lifetimes. Granular bulk aerogels will also NANOSTRUCTURES: AN INTERDISCIPLINARY be developed for our smart pebbles" concept. APPROACH PROPERTIES Application of this inconspicuous material to an area of $400,000 interest will provide a remote sensing system for covert DOE Contact: Maurice J. Katz, (202) 5866385 chemical warfare agent production facilities, battlefield SNL Contact: Gordon Osbourn, (505) 844-8850 alert for chemical weapons release, and agricultural pesticide application and runoff. Scanning Tunneling Microscopy (STM) is a powerful tool for both characterizing and manipulating the atomic Keywords: Aerogel, Remote Sensing topographies of surfaces. For chemically-uniform model systems, e.g. clean Si surfaces, STM can provide 329. SMART INTERFACE BONDING ALLOYS considerable scientific insights. However, STM has (SIBA): TAILORING THIN FILM MECHANICAL typically been unable to provide unambiguous chemical PROPERTIES recognition of atomic sites in many technologically $455,000 relevant, but chemically heterogeneoous systems. This DOE Contact: Maurice J. Katz, (202) 586-6385 limitation is due to several problems: (1) There are no SNL Contact: Stephen Foiles, (925) 294-2898 direct means for verifying proposed STM atomic identifications, and no theoretical guidance on what The use of the newly discovered strain-stabilized 2-D multivariate STM features would best characterize the interfacial alloys as smart interface bonding alloys atoms; (2) It is difficult to directly observe chemical (SIBA) is being explored. These materials are being information by inspecting individual STM images, and used as templates for the heteroepitaxial growth of this-chemical information is 'buried" among the metallic thin films. SIBA are formed by two metallic multiple-bias images; (3) STM tip structures have components which mix at an interface to relieve strain important yet poorly understood effects on STM data, and prevent dislocations from forming in subsequent and these tips often change due to tip-surface thin film growth. The composition of the SIBA is interactions during imaging. This project is developing determined locally by the amount of strain, and theoretical and experimental underpinnings to address therefore can react "smartly' to areas of the highest the three issues above with the goal of enabling strain to relieve dislocations. In this way, SIBA can be unambiquous, computer-based identification of atomic used to tailor the dislocation structure of thin films. sites in multivariate STM imagery, focusing on heterogeneous III-V semiconductor materials and This project includes growth, characterization and atomically-engineered nanostructures. The project has modeling of films grown using SIBA templates. several subtasks: (1) develop the first 'database" of Characterization includes atomic imaging of the multivariate STM spectral features (i.e., the analogue of dislocations structure, measurement of the mechanical satellite "ground truth" spectra); (2) study the effects of properties of the film using interface force microscopy different tip states on the STM spectral features and (IFM) and the nanoindenter, and measurement of the attempt to establish procedures for computationally electronic structure of the SIBA with synchrotron removing or minimizing variable-tip effects; (3) use photoemission. Resistance of films to sulfidation and pattern recognition of STM spectral imagery, based on oxidation is also being examined. The Paragon parallel the results of A and B tasks, to map out the atomic processing computer is being used to calculate the scale chemical structure of selected cleaved (119) III-V structure of the SIBA and thin films in order to develop surfaces. The alloy ordering and interfacial structure of ability to predict and tailor SIBA and thin film behavior. III-V structures of current programmatic interest for IR device applications is being studied. This work will lead to the development of a new class of thin film materials with properties tailored by varying the Keywords: Nanostructures, STM composition of the SIBA, serving as a buffer layer to relieve the strain between the substrate and the thin 331. ENABLING SCIENCE & TECHNOLOGY FOR film. Such films will have improved mechanical and COLD SPRAY DIRECT FABRICATION corrosion resistance allowing application as protective PROPERTIES barriers for weapons applications. They will also exhibit $330,000 enhanced electrical conductivity and reduced DOE Contact: Maurice J. Katz, (202) 5866385 electromigration making them particularly suitable for SNL Contact: Mark Smith, (505) 845-3256 application as interconnects and other electronic needs. Direct Fabrication is envisioned as a rapid, agile, economical process technology that additively builds up Keywords: Joining, Smart Materials a net or near-net shaped component made of one or more materials directly from a computer model; such technology would be of enormous benefit to SNL's core National Security Mission and U.S. industry. Cold Spray Processing (CSP) is a recently discovered, poorly understood, Russian technology that can rapidly deposit

159 Office of Fossil Energy

(mm/sec) metals, polymers, and composites at indispensable in developing reliable, atomic-scale, temperatures < 200°C by accelerating powder particles mechanistic models. up to 600-1000 m/s in a supersonic compressed air or gas jet. The Russians have used CSP for high-rate Keywords: AT-STM, LEEM, MPC coating deposition, but no one has attempted direct fabrication via CSP One can envision a radical new 333. FREEFORMING OF CERAMICS AND fabrication technology in which a highly focused CSP COMPOSITES FROM COLLOIDAL SLURRIES particle 'beam' is combined with a multi-axis robotic $450,000 motion system in order to spray-fabricate a single- or DOE Contact: Maurice J. Katz, (202) 586-6385 multi-material component directly from a computer SNL Contact: Michael Cieslak, (505) 845-9144 model. CSP build rates should be substantially higher than present layer-wise direct fabrication techniques This project is developing a model-based direct freeform and, since CSP particles are never fully melted, superior fabrication technique for ceramic, metal, or graded surface finishes, microstructures, and properties might composite components. These components are be achieved (finer grain size, no brittle phases, minimal fabricated without molds or tooling by building two- oxidation, less residual stress, etc.). With CSP, one dimensional layers into three-dimensional shapes by might also deposit functionally graded or layered dispensing colloidal suspensions through an orifice. Any materials at low temperatures, thus eliminating joining conceivable two-dimensional pattern may be "written" operations, simplifying design/fabrication, reducing part layer by layer into a three-dimensional shape. Initial counts, and decreasing stress cracking. (For example, experiments have demonstrated technique feasibility for aluminum has been CSP-deposited directly onto simple aluminum oxide shapes. The goal is to develop smooth, unprepared glass with excellent adhesion.) model-based processing rules that will aid in the CSP may also be an environmentally friendly alternative development of slurries with the appropriate rheology, to problem technologies, such as copper electroplating density, and drying kinetics to insure process success and soldering or painting of aircraft, weapons, etc. for a variety of ceramics and composites. Software and equipment development is also essential for precise This project explores the use of cold spray processing control of layer thickness and feature resolution. for direct fabrication of simple proof-of-concept shapes. Development of this technique into a manufacturing Keywords: Cold Spray Processing, Direct Fabrication process requires: computer simulations of the relevant physical phenomena; materials expertise for tailoring 332. ATOMIC-LEVEL STUDIES OF SURFACTANT- colloidal slurry properties and processing dissimilar DIRECTED MATERIALS GROWTH materials; software and equipment expertise for CAD $400,000 model conversion; and, robotics expertise for process DOE Contact: Maurice J. Katz, (202) 586-6385 optimization and incorporation of knowledge-based SNL Contact: Terry Michalske, (505) 844-5829 processing capabilities with closed loop sensor-based control. This project is investigating converting surface impurities from a nuisance to a systematically This work directly impacts the production of neutron applicable nano-fabrication tool. Combining Sandia's tubes (MC4277, MC4300 and RP2) and ceramic fixtures special facilities, including the 'atom-tracker" Scanning for switch tubes (MC3859). Tunneling Microscope (AT-STM), Low Energy Electron Microscopy (LEEM), and Massively Parallel Keywords: Ceramics, Composites, Freeforming Computation (MPC), the objective is to learn how common adsorbed atoms ('surfactants') can be used to 334. LASER ASSISTED ARC WELDING FOR manipulate and direct thin-film growth, and to develop a ALUMINUM ALLOYS 'surfactant toolkit' that enables production of either $200,000 atomically flat or 3-dimensionally nano-structured DOE Contact: Maurice J. Katz, (202) 586-6385 surfaces. The approach is to start with model systems, SNL Contact: Brian Damkroger (505) 845-3592 studying surfactant-modified diffusion on and near metal and semiconductor surfaces, and integrating real- At this time, there exists a strong need in the defense time experimental and advanced computational programs, automotive, aerospace and transportation modeling capabilities. The AT-STM is being used to industries for a rapid, robust, high quality process for study H-assisted Si adatom diffusion on Si(001), and welding aluminum alloys, especially for relatively thin the LEEM to investigate both H-assisted step gauge product. While laser beam welding is widely fluctuations on the same surface and O-assisted island applied in these industries it has not proved valuable for growth on Pt(111). Ge segregation versus adsorbate aluminum because of problems with reflectivity and overlayer coverage is being investigated in Si-Ge alloys weld joint variability. Gas metal arc welding (GMAW) is via novel surface stress measurements. Theoretical widely used for thick section aluminum welding because efforts are closely coupled to experiments-MPC is the process can compensate for part fit-up and metallurgical deficiencies. Under this project a new welding process is being developed by combining

160 Office of Fossil Energy

together a fiber optic delivered pulsed Nd:YAG laser MATERIALS PROPERTIES, BEHAVIOR, with a miniaturized GMAW system. The new laser CHARACTERIZATION OR TESTING assisted arc welding (LAAW) process couples the process advantages of these two unique heat sources 336. AGING AND RELIABILITY and will also enable process capabilities never before $1,997,000 envisioned in arc welding. These two heat sources are DOE Contact: Robin Staffin, (202) 586-7590 being combined in a compact (likely patentable) device SNL Contact: Richard J. Salzbrenner, that can be manipulated on the end of a robotic arm. (505) 844-9408 The focused pulsed Nd:YAG laser beam assures deep weld penetration and ablative removal of the tenacious The Materials Aging and Reliability and Aging Project aluminum oxide. The arc is focused and located by the advances the understanding of the microstructural metal vapor and gas ions generated by the high mechanisms which control the aging, reliability, and intensity laser beam. Increased arc stability is performance of materials. The selection of subprojects anticipated since the gas metal arc is known to be is based on the risk (likelihood vs. consequence) of the stabilized by thermal ionization of the shielding gas. The failure of a specific material to weapon performance or project is a System of Laboratories (SOL) collaboration surety. All subprojects seek to develop fundamentally- among ORNL, INEEL and SNL. These three based prediction capability to determine the effects of laboratories have distinguished themselves for their aging on the performance and reliability of non-nuclear contributions to the science and technology of materials materials used in nuclear weapons. This project joining. The team established through this SOL supports materials science work that is collaborative interaction should allow the U.S. to successfully with other research programs to develop predictive compete with international entities, such as Germany's capability that can be applied to the enduring stockpile. Fraunhofer Institute, in developing (and hence owning) advanced joining technologies for commercially critical Keywords: Aging, Reliability markets. 337. NANOSCALE STRUCTURES AND Keywords: Laser-Assisted Arc Welding PHENOMENA $1,070,000 335. SYSTEM STUDIES IN ELECTROCHEMICAL DOE Contact: Robin Staffin, (202) 586-7590 PROCESSING PROPERTIES SNL Contact: Michael I. Baskes, (925) 294-3226 $100,000 DOE Contact: Maurice J. Katz, (202) 586-6385 The Nanoscale Structures and Phenomena Project SNL Contact: Martin Carr, (505) 844-6070 encompasses research on all classes of materials whose properties depend on phenomena unique to The objective of this project is to develop physical small (< 1 micron) size. Properties are studied in order models and associated analytical tools that will allow a of decreasing interest and include mechanical, number of electrochemical processes of interest to be electrical, magnetic, and optical. Synthesis of both more effectively characterized. In addition to the materials and structures, materials characterization, availability of new models and tools, the important and performance are linked using appropriate theory contribution of this activity is the determination of the and modeling of model systems. Emphasis is placed on conceptual feasibility of using this type of approach to obtaining an understanding of controlling mechanisms solve engineering-level electrochemical problems. in these model systems and extending this Because of the limited scope of the project, two very understanding to predictions of complex materials and specific processes have been selected for detailed devices. study. Four primary tasks are included: (1) detailed analysis of relevant literature information, (2) planning Keywords: Nanoscale Structures, Nanoscale and execution of required experiments, (3) formulation Phenomena of analytical models, and (4) laboratory demonstration/ validation of the models using untested configuration. 338. APPLICATIONS-DRIVEN INTERDISCIPLINARY RESEARCH Keywords: Electrochemical Processing, Modeling $885,000 DOE Contact: Robin Staffin, (202) 586-7590 SNL Contact: Samuel T. Picraux, (505) 844-5829 The Applications-Driven Interdisciplinary Research works with the National Security sector [including Micromechanical (IMEMS) reliability and high-reliability neutron tube fabrication and mid-IR based chemical sensors] and focuses on collaboration. Research

161 Office of Fossil Energy specifically focuses on National Security and building on bandgap structures (PBG), and to exploit its unique emerging technology core capabilities. properties for the design and implementation of photonic devices on a nano-meter length scale for the Keywords: Sensors, Micromechanical, Infrared control and confinement of light. The low loss, highly reflective and quantum interference nature of a PBG 339. MATERIALS STABILITY AND THIN COATINGS material makes it one of the most promising candidates $2,483,000 for realizing an extremely high-Q resonant cavity, DOE Contact: Robin Staffin, (202) 586-7590 >100,000, for optoelectronic applications and for the SNL Contact: Terry A. Michalske, (505) 844-5829 exploration of novel photonic physics, such as photonic localization, tunneling and modification of spontaneous The Materials Stability Thin Coatings research seeks to emission rate. Moreover, the photonic bandgap concept develop and apply atomic- and molecular-level affords a new opportunity to design and tailor photonic microscopies, spectroscopies, and theoretical models to properties in very much the same way one manipulates, examine fundamental materials processes that control or bandgap engineers, electronic properties through phenomena, including: interfacial adhesion, lubrication, modern epitaxy. wear thermal stability, thin-film and surface kinetics, radiation effects, corrosion, hydrogen effects, curing, Keywords: Photonics, Bandgap, Epitaxy fracture, and chemical and physical vapor deposition processes. Also, this research seeks to develop a 342. MODEL DETERMINATION AND VALIDATION scientific basis for design, manufacture, and application FOR REACTIVE WETTING PROCESSES of small, smart products; new models to predict useful $351,000 lifetimes for currently used materials and structures; DOE Contact: Maurice J. Katz, (202) 586-6385 and transfers of technology regarding degradation of SNL Contact: Frederick Yost, (505) 844-5278 resistant/stable materials to U.S. This work was undertaken to develop a computational Keywords: Coatings, Stability model of reactive wetting processes. Although wetting and spreading have been studied in great detail, most of 340. CATALYTIC MEMBRANE SENSORS this work pertains only to inert or nonreactive wetting. $361,600 Inert wetting is driven by an imbalance of surface DOE Contact: Maurice J. Katz, (202) 586-6385 tension forces with no other interaction between the SNL Contact: William Hammetter, wetting liquid and the substrate. In reactive wetting (505) 272-7603 other processes such as diffusion, intermetallic reactions, and environmental reactions may drive or The goal of this project is to develop a fundamentally hinder the continuous advance of the wetting front. new catalytic membrane-based sensor (CMS) with Additional aspects of reactive wetting are being enhanced sensitivity and specificity through investigated to determine the driving and dissipation modification of an SNL-developed Pd/Ni-based forces that are thought to control the spreading behavior hydrogen sensor. This will be accomplished through in reactive wetting systems. With this understanding overlays of size selective gas separation membrane and wetting problems of technological significance can be ion exchangeable titanate catalyst. The goal is to controlled and processes can be improved. process these CMS elements into an array that utilizes different catalysts and membranes. This will enable Keywords: Wetting, Computation significant improvement of both the selectivity and specificity via pattern recognition methodologies. In 343. ULTRA-HARD MULTILAYER COATINGS FY 1997, the project met the following milestones PROPERTIES toward the synthesis and processing of these CMSs: $472,000 (1) synthesis and characterization of double alkoxides, DOE Contact: Maurice J. Katz, (202) 586-6385 (2) membrane modified sensor (H2 sensor), SNL Contact: Ellen Stechel, (505) 844-2436 (3) catalytically active HTO or HTO-like layer on a membrane, (4) catalytic adjustability by ion exchange, This project is exploring the production of ceramic and (5) catalyst layer on the sensor. multilayer structures that are potentially harder than any natural or artificial material. Diamond and cubic boron Keywords: Catalysis, Membranes, Sensors nitride (cBN) are the two hardest substances known to man. Numerous proven technologies rely on the 341. PHOTONIC BAND GAP STRUCTURES AS A superior mechanical properties of these materials. The GATEWAY TO NANO-PHOTONICS question arises: Is it possible to manufacture a material $375,000 that is harder than diamond? In theory, the answer is DOE Contact: Maurice J. Katz, (202) 586-6385 yes. Experiment indicates that properly grown multilayer SNL Contact: Adelbert Owyoung, (505) 844-5481 coatings of two materials are harder than either of the materials making up the individual layers. The increase The goal of this project is to explore the fundamental in hardness is mainly due to the resistance of disloca- physics of a new class of photonic materials, photonic tion flow across the interfaces between phases of

162 Office of Fossil Energy different elasticity. This experimental fact leads to the level engineering of its local structural environment in a possibility that a new class of ultra-hard materials- nanocomposite, optical ceramic host material. This harder than diamond-can be made by growing the program examines the influence of nanoscale hetero- appropriate multilayer film. geneities on ion-ion and ion-lattice energy transfer dynamics through atomic-level engineering of the RE This project uses a combination of growth, analysis and ion local environment. Both direct optical evaluation of theoretical modeling capabilities at Sandia that could the dopant behavior and theoretical structural modeling possibly lead to a revolutionary jump in both materials and simulation were employed evaluate these novel understanding and performance-a material harder host materials. The local atomic structure in the vicinity than diamond. of RE dopants was successfully modeled using a powerful Sandia-developed (QUEST) computational Keywords: Multilayer, Ultrahard approach based on local density functional theory. In AI203, this technique is being extended to model the 344. MOLECULAR-SCALE LUBRICANTS FOR difference in tetrahedral versus octahedral site MICROMACHINE APPLICATIONS symmetry on the density of electronic and vibrational $475,000 states, to allow the investigation of a variety of dopant DOE Contact: Maurice J. Katz, (202) 586-6385 site types characteristic of multiphase hosts (e.g., SNL Contact: Terry Michalske, (505) 844-5829 interfaces and clusters). This work will result in a new, computer-based, predictive materials modeling The nature of this work is to develop the physics and capability in both single and multiphase candidate chemistry base for designing molecular-scale lubricants hosts, before fabrication, and will yield an improved for the reduction of friction- and stiction-induced failure class of materials at the junction between fundamental in silicon micromachines. The approach is tailoring the solid-state physics and nanophase science to enable molecular properties of lubricants, applying local probes RE optics in photonic integrated circuits. that can directly monitor the response of lubricants in contact conditions, and evaluating the performance of Keywords: Energy Transfer, Optics, Ceramics model lubricants on micromachine test structures specifically designed for friction and stiction studies. 346. INTEGRATED THIN FILM STRUCTURES FOR IR IMAGING PROPERTIES Model lubricants under investigation are the silane $430,000 coupling agents that form self-assembling monolayer DOE Contact: Maurice J. Katz, (202) 586-6385 (SAM) films on native oxide silicon surfaces. With SNL Contact: Alan Hurd, (505) 272-7642 atomic force microscopy (AFM) and interfacial force microscopy (IFM), the role of chain length, chemical Uncooled pyroelectric IR imaging systems, such as end group, and chain structures on the frictional and night vision goggles, offer important strategic adhesive properties of the SAM films is being examined, advantages in battlefield scenarios and reconnaissance surveys. Unfortunately, the current technology for Using a recently-completed scanning near-field optical fabricating these devices is limited by low throughput microscope (SNOM), the goal is to provide the first-ever and high cost which ultimately limit the availability of simultaneous correlation between SAM film structure these sensor devices. and dynamic mechanical response. Emission from dilute concentrations of "guest" chromophores, whose This project is developing an alternative design for orientation(s) are sensitive to lateral- and normal-force- pyroelectric IR imaging sensors that utilizes a multilayer induced changes in the lubricating film structure will be thin film deposition scheme to create a fully integrated monitored. These AFM, IFM, and SNOM measurements thin film element on an active silicon substrate for the will form a very important link for molecular dynamics first time. The approach combines a thin film simulations, that, in turn, should be able to predict pyroelectric imaging element with a thermally insulating micromachine performance under all conditions. SiO 2 aerogel thin film to produce a new type of uncooled IR sensor that offers significantly higher Keywords: Lubricants, Micromachines thermal, spatial, and temporal resolutions at a substantially lower cost per unit. 345. UNDERSTANDING AND CONTROL OF ENERGY TRANSFER MECHANISMS IN Keywords: Thin Films, IR Imaging OPTICAL CERAMICS PROPERTIES $400,000 DOE Contact: Maurice J. Katz, (202) 586-6385 SNL Contact: Clifford Renschler, (505) 844-0324

A radically new material strategy for rare-earth (RE) hosts was developed. In this approach, the optical performance of the dopant is modified through atomic-

163 Office of Fossil Energy

347. THE INITIATION AND PROPAGATION OF being utilized to develop contiguous, high surface area NANO-SCALE CRACKS AT AN polymers as nanoporous supports for ultra-efficient ADHESIVE/SOLID INTERFACE PROPERTIES separations. These materials are being evaluated using $400,000 capillary electrochromatography (CEC) as a test bed. DOE Contact: Maurice J. Katz, (202) 586-6385 The interaction of functionalized surfaces of these SNL Contact: Wendy Cieslak, (505) 844-8633 supports with analytes, propelled by the electroosmotic flow (EOF), is being quantified in terms of separation This project is investigating submicron debonding efficiency and selectivity. Dramatic gains enabling processes at polymer/solid interfaces with a miniaturization are anticipated with increased efficiency combination of continuum stress analysis, molecular and selectivity of CEC. The goal is to engineer an open dynamics (MD) simulations, and a new experimental and interconnected network where every nanopore approach. Each component of this program is designed functions as a CEC column. These enhancements are to provide complementary information with the goal of not possible in conventional chromatographic methods. bridging the gap between molecular and continuum These new solid supports, which are cast as fluid descriptions. The objective is a validated, molecular-to- solutions and cured to monolithic polymer structures, continuum fracture theory. Despite significant progress are being integrated into micro-machined grooves as made in recent years in the fields of fracture mechanics pre-prototype devices for ultra-efficient separations. and adhesion science, it is still not possible to predict Unfilled microgrooves are also being evaluated for their the lifetime of a polymer/solid interface from first inherent separation efficiencies. principles. On the continuum level, considerable headway has been made in an interfacial fracture Keywords: Nanoseparation, Polymers mechanics approach for preexisting macroscopic cracks between linear elastic materials. Little is known, 349. FUNDAMENTAL ASPECTS OF however, about modeling cracks on a micron or MICROMACHINE RELIABILITY submicron level, how microcracks develop into $350,000 macroscopic cracks, or about length scale limitations on DOE Contact: Maurice J. Katz, (202) 586-6385 the use of a continuum analysis. Furthermore, there is SNL Contact: Terry Michalske, (505) 844-5829 an interphase region with property gradients between the two bulk materials. The effect of interface structure A fundamental basis for designing micromechanical and molecular properties on fracture mechanics devices with high yield, reliable performance and long parameters is unknown. On the molecular scale, much life is lacking. Mechanical design tools for macro-scale is known about polymer dynamics, the origin of machines relate reliability to inertial forces. However, viscoelastic behavior and relaxation phenomena, and the performance of micron-scale structures of high the behavior of polymers near surfaces. Yet it is not aspect ratio is dominated by surface forces. The clear how stress concentrations develop on a molecular technical goal of this project is to use experimental scale in an imperfect thermoset polymer, or how reliability results obtained directly from micromachined nanoscale inhomogeneities grow into microcracks under test structures to develop and verify mechanics models stress. An understanding of the link between the containing interaction terms appropriate to the micron- molecular and the continuum levels is required before scale (e.g. capillarity, van der Waals forces, electro- the goal of a truly comprehensive model of fracture can statics, etc.). Issues to be addressed include auto- be approached. Such a theory would allow the adhesion (stiction), friction and wear. Microbridge prediction of lifetimes given the detailed interface structures with varying geometry and surface properties structure, material properties, and the thermal history, (roughness, chemical coatings etc.) Are being designed and would aid greatly in the design of interfaces that are and built. Deformations are being monitored by more resistant to aging. interferometry in an environmental chamber. Finite element models incorporating new surface elements are Keywords: Nanoscale, Interface, Adhesive being developed, verified and refined by comparing against experimental results. An additional objective is 348. MONOLITHIC STRUCTURES FOR to investigate friction and wear using smart micro- NANOSEPARATION PROPERTIES machined structures that enable self-diagnosis by $339,000 electrical monitoring of capacitance and Q factor DOE Contact: Maurice J. Katz, (202) 586-6385 changes. Optical detection technique is being explored. SNL Contact: James Wang, (925) 294-2786 Dynamical response models incorporating internal friction terms as well as damping are being verified and Miniaturization in detection and separation technologies refined using experimental results. Friction due to requires easily built, rugged devices based on materials energy loss at rubbing surfaces can then be extracted. that have well understood interactions with analytes at the molecular level. The goal of this project is to design This project is developing a new tool set based on an such materials for state-of-the-art separation science, experimental and theoretical foundation. The tool set understand their structure/function relationships, and fabricate them into useful devices. Sandia expertise in the synthesis of micro- and nanoporous materials is

164 Office of Fossil Energy can be used to calculate and characterize reliability of interesting properties, including large catalytic activity, micromachines for integrated microsystem applications. room temperature luminescence, size dependent bandgaps, etc., and are sufficiently monodisperse that Keywords: Micromachine, Reliability size-dependent cluster properties can be easily resolved. However, these clusters are currently stable 350. INTELLIGENT POLYMERS FOR NANODEVICE only in the reaction bath. Second, Sandia has PERFORMANCE CONTROL developed an expertise in synthesizing bulk periodic $439,000 mesoporous materials by templating silica around liquid DOE Contact: Maurice J. Katz, (202) 586-6385 crystalline surfactant assemblies. These surfactant- SNL Contact: Clifford Renschler (505) 844-0324 templated porous materials (STPMs) are similar to zeolites, but the unit cell size is 40A versus the 4-8A This project is developing a revolutionary enabling typical for zeolites. These are the first periodic materials technology for the accurate, predictable manipulation of whose uniform pore size is commensurate with the the fundamental optical, electrical and theological typical dimensions of quantum dots. These new properties of a new class of intelligent polymers. Their materials should be an ideal matrix for quantum dots; potential for write-once memories and nanoscale moreover, the quantum dots should form a highly "device on command" capability could find application in periodic array, which may give rise to a host of new reduced size parts (WPP) and intelligent manufacturing coherent phenomena. The goal of this project is to technologies, and compartmentalized activities at synthesize a new class of materials, "Quantum Dot Sandia and in other government agencies (use control, Arrays" (QDAs), that consists of metal or semiconductor tamper detection). The autonomous response polymers clusters periodically arrayed in an isolating silica matrix. will remain passive prior to stimulation from specific Such cluster-based materials will have unique optical, light or heat sources, when they will undergo changes in catalytic, and dielectric properties: gold clusters in silica morphology, conductivity or refractive index in response would give a high dielectric material for super- to the stimuli. Existing materials are limited to capacitors; low work function clusters could make a laboratory-scale manipulation of polymer conductivity good field emitter; luminescent silicon clusters could with ill-defined thermally- or photochemically-initiated make optical arrays; supported nanocluster catalysts changes to the polymer's chemical structure. The could be made as thin films. approach of this project provides enhanced, well- defined control of polymer properties through molecular Keywords: Quantum Dot, Nanocluster scale design of polymer structure. Materials are synthesized to covalently incorporate energetic DEVICE OR COMPONENT FABRICATION, chemical functionalities within the polymers' molecular BEHAVIOR OR TESTING structures. Appropriate energetic groups are then selected as monomers from molecular modeling of the 352. WIDE-BANDGAP COMPOUND energetic group's kinetic and thermodynamic response SEMICONDUCTORS TO ENABLE NOVEL to heat and light, and the compatibility of the groups to SEMICONDUCTOR DEVICES PROJECT co-monomers bearing latent reactivity. The energetic $290,000 groups are incorporated as terminal groups or as blocks DOE Contact: Maurice J. Katz, (202) 586-6385 of repeat units within the polymer backbone by SNL Contact: Jeffrey Nelson, (505) 844-4395 employing living polymerization techniques including Ring Opening Metathesis Polymerization (ROMP). . This project is an interdisciplinary investigation into the Energetic group decomposition, stimulated from a growth and physical properties of wide-bandgap specific source, indirectly activates the reactive repeat compound semiconductors for the purpose of enabling units, resulting in dramatic changes in macroscopic both optoelectronic and microelectronic device properties including refractive index, electrical development. The AlGaInN material system is widely conductivity or material bulk morphology. considered to be essential to the development of a wide array of UV and blue optical devices as well as high- Keywords: Polymers, Nanodevices temperature microelectronics. A critical limiting factor in the demonstration of advanced Ill-N based devices is 351. QUANTUM DOT ARRAYS the lack of an in-depth understanding of the physics and $400,000 chemistry that govern the unique properties of these DOE Contact: Maurice J. Katz, (202) 586-6385 materials. This work focuses on two important areas in SNL Contact: George Samara the development of these materials. A portion of the effort concentrates on understanding the growth of III-N This project integrates two areas of Sandia research to materials by gas-source molecular beam epitaxy fabricate new molecularly engineered, cluster-based, (GSMBE), specifically the effects of substrate nanocomposite materials. First, Sandia has patented preparation, substrate temperature, VIIIl ratio, and the inverse micellar synthesis of highly monodisperse growth rate on the nucleation and growth of AIGaInN on metal and semiconductor nanoclusters, or "quantum 6H-SiC (0001) surfaces using in situ reflection high- dots." These 10-100 A nanoclusters have many energy electron diffraction (RHEED), reflection mass

165 Office of Fossil Energy spectroscopy (REMS), and scanning tunneling 354. SURFACE MICROMACHINED FLEXURAL microscopy (STM). In combination with efforts to study PLATE WAVE DEVICE INTEGRATED ON crystal growth processes in these materials, the SILICON physical properties of the AIGaInN material system are $525,000 being investigated. Analytical investigations include DOE Contact: Maurice J. Katz, (202) 586-6385 calculations to determine bandstructure and SNL Contact: Stephen Martin, (505) 844-9723 development of a model for optical gain and lasing which will include an exact treatment of Coulomb Small, reliable chemical sensors are needed for a wide effects. Steady state and time-resolved luminescence is range of applications, such as, weapons state-of-health used to evaluate the nature of defect states in these monitoring, nonproliferation activities and manufac- materials as well as to study the excitonic properties turing emission monitoring. Advantages of a flexural which are expected to be enhanced for wide-bandgap plate wave (FPW) architecture for these sensors include semiconductors. Magnetoluminescence experiments improved sensitivity, reduction in operating frequency to determine energy dispersion and effective masses and be compatible with standard digital microelectronics and these results are directly compared with bandstructure sensing in liquid media. This project investigates calculations. Another aspect of the work is an fabrication of these miniaturized, high reliability devices, evaluation of how various processing techniques which which requires successful execution and integration of are relevant for device fabrication, such as post-growth three technologies: acoustic sensor design; Si surface annealing, reactive ion etching and implantation, affect micromachining; and high quality piezoelectric thin film the optical and electronic properties of the III-N deposition. materials. Keywords: Micromachines, Silicon Keywords: MBE, HEED, REMS, STM 355. MODELING ELECTRODEPOSITION FOR 353. SCANNING PROBE-BASED PROCESSES FOR METAL MICRODEVICE FABRICATION NANOMETER-SCALE DEVICE FABRICATION PROPERTIES $442,600 $265,000 DOE Contact: Maurice J. Katz, (202) 586-6385 DOE Contact: Maurice J. Katz, (202) 586-6385 SNL Contact: Terry Michalske, (505) 844-5829 SNL Contact: Jill Hruby, (925) 294-2596

Nanometer-scale electronic device technology requires LIGA, an acronym from the German words for a novel physics base that includes fabrication lithography, electroforming, and molding, is a promising processes, characterization techniques and materials new process for producing metal microdevices having properties allowing reliable performance of devices at micron to millimeter features. Currently under worldwide this very small length scale. This program integrates development, this process offers a means to manu- and expands Sandia's expertise in scanning-probe facture high resolution, high aspect-ratio devices based fabrication and characterization of nanostructures including microscale valves, motors, solenoid actuators, with capabilities in microelectronic fabrication to and gear trains. Most research in LIGA has focused on produce fully accessible nanostructures for electronic the lithography process used to produce LIGA molds. evaluation. The objective is an order of magnitude Filling these molds by electrodeposition has received decrease in feature size compared to conventional much less attention, despite several serious problems. fabrication technology. Approaches to nanostructure Device-scale voids in the deposited metal occur fabrication using scanning probe-based (STM, AFM) frequently and often without apparent cause. These processes in combination with extensive device problems are likely due to the depletion of metal ions fabrication are being explored. For prototype device and the accumulation of hydrogen in the stagnant layer structures critical nanoscale components are being between the top and bottom of the mold. The presence integrated with conventional test structures to allow full of this diffusion layer distinguishes LIGA electro- electrical accessibility. Two approaches to deposition from traditional electroplating and nanostructure fabrication are being explored: electroforming processes. investigation of molecular layer resists based on simple adsorbed atoms and molecules which can be patterned To help understand and optimize the electroforming by electron induced desorption or reaction, and portion of the LIGA process, this project is developing a development of a more general AFM-based one-dimensional numerical model describing the nanolithographic capability, based on anodic oxidation electrodeposition of metal into high aspect-ratio molds under an AFM tip. In parallel with these fabrication having lateral dimensions on the micron scale. To guide approaches, low temperature electrical measurements model development, and later to validate this model, a are being performed, and selected nanoelectronic series of one and two-dimensional laboratory devices are being fabricated and characterized. experiments are being coordinated.

Keywords: Nanoscale, Device Fabrication Keywords: Micromachines, Electrodeposition

166 Office of Fossil Energy

INSTRUMENTATION AND FACILITIES models must be built upon understanding of the elementary events involved in surface damage and 356. ADVANCED ANALYTICAL TECHNIQUES mobility. The project is developing a new approach to $998,000 examine the fundamental mechanisms controlling DOE Contact: Robin Staffin, (202) 586-7590 physico-chemical surface stability that combines: SNL Contact: Julia M. Phillips, (505) 844-1071 (1) atomic-scale control of surface contact forces and displacements under well controlled adsorbate The Advanced Analytical Techniques Project supports conditions using the Interfacial Force Microscope; the development of advanced methods of characterizing (2) atomic-level imaging of surface and near-surface materials structure and providing chemical analysis. structure and defects using Field Ion Microscopy and Each of the relatively independent subprojects is Transmission Electron Microscopy; and (3) first- directed towards advancing the state-of-the-art in principles modeling of the effect surface stress on materials characterization by developing new adsorbate bonding interactions and the subsequent capabilities for extracting information about materials generation of surface damage. through the development of new hardware or data analysis techniques. Each project must offer at least Keywords: Stability, Surface, Wear one of the following: (1) improvement in Sandia's ability to monitor the nuclear stockpile or nuclear weapon ...I...'- ' E. A INA production or maintenance processes, or (2) the ... O .''...... capability to perform failure analysis on weapons LABO ORY components, materials, or subsystems. 'lill I lt llll

Keywords: Chemical Analysis, Characterization MATERIALS PREPARATION, SYNTHESIS, DEPOSITION, GROWTH OR FORMING 357. NANOSTRUCTURES, ADVANCED MATERIALS, AND ION BEAM SCIENCES 359. ENGINEERED NANOSTRUCTURE LAMINATES $2,792,000 $2,000,000 DOE Contact: Robin Staffin, (202) 586-7590 DOE Contact: G. J. D'Alessio, (301) 9036688 SNL Contact: George A. Samara, (505) 844-6653 LLNL Contact: Troy W. Barbee, Jr., (925) 423-7796 This research keeps Sandia at the forefront of experimental and theoretical materials science relevant Multilayers are man-made materials in which to National Security needs and includes experiment and composition and structure are varied in a controlled theory of new materials (e.g., nanoclusters, manner in one dimension during synthesis. Individual nanostructures, polymeric ferro electrics, amorphous layers are formed using atom by atom processes diamond films, and shock wave-induced phenomena) of (physical vapor deposition) and may have thicknesses proven or potential application in current or future of from one monolayer (0.2 nm) to hundreds of mono- weapon systems. The program also develops new ion- layers (>100 nm). At this time more than 75 of the 92 beam based tools required to fully characterize or naturally occurring elements have been incorporated in modify these new materials systems (e.g., radiation multilayers in elemental form or as components of effects microscopy) and new computational tools for alloys or compounds. In this work deposits containing improved structural/electronic/photonic property up to 225,000 layers of each of two materials to form up simulations. to 500p thick samples have been synthesized for mechanical property studies of multilayer structures. Keywords: Nanostructures, Ion Beam These unique man-made materials have demonstrated 358. PHYSICO-CHEMICAL STABILITY OF SOLID extremely high mechanical performance as a result of SURFACES the inherent ability to control both composition and $413,000 structure at the near atomic level. Also, mechanically DOE Contact: Maurice J. Katz, (202) 586-6385 active flaws that often limit mechanical performance are SNL Contact: Terry Michalske, (505) 844-5829 controllable so that the full potential of the structural control available with multilayer materials is accessible. The application of physico-chemical phenomena to Systematic studies of a few multilayer structures have either increase machinability of hard materials, improve resulted in free-standing foils with strengths the wear resistance of cutting surfaces, or enhance approaching those of whiskers, approximately 70 sintering of particle compacts can have large economic percent of theory. Also, new mechanisms for impact on technologies ranging from materials forming mechanically strengthening materials are accessible processes to oil well drilling. Unfortunately, the broad with nanostructure laminates. application of these physico-chemical principles is limited by the ability to predict the optimum conditions Applications now under development include: coatings for a wide variety of materials surfaces. Predictive for aircraft gas turbine engines; EUV, soft X-ray and X-

167 Office of Fossil Energy

ray optics spectroscopy and imaging; high performance 362. ENERGETIC MATERIALS STRATEGIC capacitors for energy storage; capacitor structures for CHEMISTRY industrial applications; high performance tribological $350,000' coatings; strength materials; integrated circuit DOE Contact: Bharat Agraval, (301) 903-6688 interconnects; machine tool coatings; projection X-ray LLNL Contact: R. L. Simpson, (925) 423-0379 lithography optics. Vicarious nucleophilic substitution chemistry is being Keywords: Thin Films, Multilayer Technology used to synthesize energetic materials. New explosive molecules are being synthesized. Alternate routes to 360. SOL GEL COATINGS existing molecules, such as TATB, have been $335,000 developed. DOE Contact: G. J. D'Alessio, (301) 903-6688 LLNL Contact: I. M. Thomas, (925) 423-4430 and Keywords: Examination, Explosive, Energetic, TATB J. Britten, (925) 423-7653 363. CHEETAH THERMOCHEMICAL CODE This project investigates the preparation of multilayer $190,000' sol-gel high reflection (HR) coatings using colloidal SiO2 DOE Contact: Bharat Agraval, (301) 903-6688 with either HfO2 or ZrO2. The incorporation of an LLNL Contact: R. L. Simpson, (925) 423-0379 organic polymer binder such as polyvinyl alcohol or polyvinyl pyrolidinone into the high index component A thermochemical code for the prediction of detonation has resulted in an increase in the damage threshold and performance is being developed. In addition to a decrease in the number of layer pairs required for high detonation performance, thermochemical calculations of reflection. A laboratory size meniscus coater was impetus and specific impulse for propellant applications evaluated and found to produce mirrors of high optical may also be made. performance and adequate damage threshold. This is now the preferred method of application, and a large Keywords: Examination, Explosive, Energetic, TATB machine capable of producing Beamlet and NIF size mirrors is in place. 364. EXPLOSIVES DEVELOPMENT $900,0001 Keywords: Sol Gel Coatings, Meniscus Coater, HR DOE Contact: Bharat Agraval, (301) 903-6688 Coatings LLNL Contact: R. L. Simpson, (925) 423-0379

361. KDP AND DKDP CRYSTAL DEVELOPMENT New explosives are being developed for hard target AND PRODUCTION penetrators. The goals include insensitivity to shock $4,000,000 loading and significantly higher energy density than that DOE Contact: G. J. D'Alessio, (301) 903-6688 of currently available materials. LLNL Contact: J. J. DeYoreo, (925) 423-4240 Keywords: Explosive Potassium dihydrogen phosphate (KDP) and its deuterated analog (DKDP) are important nonlinear MATERIALS PROPERTIES, BEHAVIOR, crystals which will be used both for frequency CHARACTERIZATION.OR TESTING conversion as well as for a large Pockels cell on the National Ignition Facility (NIF). These crystals are very 365. INTERFACES, ADHESION, AND BONDING expensive, due in part to the very long times required to $250,000 grow large boules (2-3 years) and the cost of D20 for DOE Contact: Iran L. Thomas, (301) 903-6688 growing DKDP. This project has developed an LLNL Contact: Wayne E. King, (925) 423-6547 alternative growth technique that dramatically increases the growth rate of these crystals. The experimental effort is producing results that are directly comparable with theoretical calculations. Planar Using this method both KDP and DKDP are being metal/metal interfaces and metal/ceramic interfaces (in grown at 10 times the rates achieved with conventional anticipation of improvements in the theory) of well methods. High quality crystals up to almost 57cm on a defined misorientations are being investigated. In order side have been grown by this method. Crystals at the to span the entire range of length scales described 10-15cm scale are being grown in order to determine above, macroscopic bicrystals a few millimeters thick, optimum hydrodynamic and regeneration conditions, with interfacial areas on the order of a square and to understand the effects of impurities and stresses centimeter, are required. In order to obtain such on the stability of the growing crystal face and the bicrystals, diffusion bonding is used. An ultra-high- performance of the crystals.

Keywords: KDP, Nonlinear Crystals, Crystallization General energetic materials-related input. This activity is jointly funded (50:50) by DOE DP and the DoD.

168 Office of Fossil Energy

vacuum diffusion bonding machine has been developed Techniques used include optical scatterometry, in parallel with this research project. spectroscopy, X-ray typography, crystal growth and chemical analysis to determine the distribution of Keywords: Interfaces, Bonding, Electronic Structure defects in crystals and their relationship to the growth process. Strain and damage have been related to 366. LASER DAMAGE: MODELING AND specific defects using these methods and the process of CHARACTERIZATION laser damage as well as laser and thermal annealing is $1,000,000 now under investigation in situ. DOE Contact: G. J. D'Alessio, (301) 903-6688 LLNL Contact: M. R. Kozlowski, (925) 424-5637 Keywords: KDP, Strain, Crystal The objective of this project is to understand the INSTRUMENTATION AND FACILITIES mechanisms for laser-induced damage in optical materials used in high-peak-power laser systems such 368. SCANNING TUNNELING MICROSCOPY (STM) as the National Ignition Facility (NIF). Materials of AND ATOMIC FORCE MICROSCOPY (AFM) primary concern are optical coatings and polished fused $250,00 silica surfaces. The primary characterization tools used DOE Contact: G. J. D'Alessio, (301) 903-6688 in the studies include Atomic Force Microscopy (AFM), LLNL Contact: W. Siekhaus, (925) 422-6884 Total internal Reflection Microscopy (TIRM), Near-field Scanning Optical Microscopy (NSOM), Secondary Ion A large stage scanning probe microscope that can Mass Spectroscopy (SIMS) and Photothermal perform scanning tunneling as well as contact and non- Microscopy (PTM). Efforts are focused on the contact atomic force microscopy on the surface of development of characterization tools that have objects as large as 6" in diameter, a small stage improved resolution and detection limits and that can modified so that it can perform non-contact AFM and differentiate between damaging and non-damaging STM as well as nano-indentation, and an ultra-high defects. vacuum instrument that can perform non-contact AFM and STM measurements and STM spectroscopy (STS) An understanding is also needed of the growth of are being used for the following studies: damage resulting from illumination pulses after the initial onset of damage. The damage growth rate Uranium Hydriding - Understanding the early stages of determines the functional lifetime of the optic in the uranium hydriding and the effect of surface impurities is laser system. The dependence of the damage growth of paramount importance in science based stockpile rate on laser wavelength, pulse length, and pulse stewardship. The UHV STM/AFM is used to determine repetition rate are being determined. Also of interest is the effect of local impurities on uranium hydriding. the influence of optic environment (air vs. Vacuum) on the damage processes. Electronic Properties of Nano-scale Particles - Nm-scale clusters various materials, deposited by laser ablation Keywords: Coatings, Atomic Force Microscopy, Laser and by evaporation in a noble gas atmosphere onto the Damage basal plane of graphite are analyzed by STM to determine their size distribution and by optical 367. KDP CHARACTERIZATION spectroscopy and electron spectroscopy to determine $1,000,000 their size-dependent optical properties and electronic DOE Contact: G. J. D'Alessio, (301) 903-6688 structure. LLNL Contact: J. J. DeYoreo, (925) 423-4240 Dissolution Rate of Uranium Oxide - The Very large, high quality crystals of potassium dissolution of uranium oxide by ground is being dihydrogen phosphate (KDP) and its deuterated determined by AFM on single crystal uranium analogue (DKDP) are required for present and oxide by monitoring the rate of recession of the advanced high power lasers in the ICF Program. The U02 surface with reference to a gold marker. performance of these crystals is limited by impurities · Combined Scanning Probe Microscopy/Nano- and strain which induces anomalous birefringence and Indentation - Used to identify the local mechanical wavefront distortion and by defects which result in laser- properties of composite materials such as fiber induced damage at low laser fluence. The level of reinforced plastics, bone-, tooth- and arterial- impurities, internal strain and the laser damage tissue from healthy and diseased arteries. threshold are the most important factors in determining Keywords: NDE, Chemical Reaction, Uranium the yield of useable plates from an 'as-grown' boule. Hydriding, Stockpile Stewardship, Uranium The goal of this project is to identify the defects which Oxide Dissolution, Nuclear Waste Disposal, are the source of strain and damage in KDP and DKDP, Etching, Cluster, Nano-indentation, understand how these defects are generated, and how Mechanical Properties, Biomaterials, Tooth, to avoid them during the growth process. Artery, Bone

169 Office of Fossil Energy

369. FATIGUE OF METAL MATRIX COMPOSITES 371. PROPERTIES OF HYDROGEN AT HIGH SHOCK $500,000 PRESSURES AND TEMPERATURES DOE Contact: Warren Chernock, (202) 586-7590 $400,000 LLNL Contact: Donald Lesuer, (925) 422-9633 DOE Contact: G. J. D'Alessio, (301) 903-6688 LLNL Contacts: William Nellis, This project involves Lawrence Livermore National (925) 422-7200 and Neil Holmes, Laboratory and General Motors. The project is studying (925) 422-7213 the mechanisms of high cycle fatigue in squeeze cast metal matrix composites. The life limiting micro- The properties of hydrogen at high pressures and structural features are being determined and the temperatures are a "Holy Grail" issue for laser fusion, processing-structure-property correlations are being condensed matter physics, and planetary physics. established. Models that can predict lifetimes will be Hydrogen in the form of deuterium-tritium is the fuel in developed. laser fusion targets; the metallization of hydrogen by electronic bandgap closure has been a key goal of Keywords: Materials Properties, Behavior, condensed matter physics since the early part of this Characterization or Testing century: and Jupiter with its 300 Earth masses is 90 percent hydrogen at high pressures and tempera- 370. MATERIALS PRODUCED WITH DYNAMIC HIGH tures. This project measures temperatures and PRESSURE electrical conductivities of cryogenic liquid hydrogen $50,000 and deuterium shock-compressed to pressures up to DOE Contact: G. J. D'Alessio, (301) 903-6688 2 Mbar (2x106 bar) and temperatures up to 5000 K with LLNL Contact: William Nellis, (925) 422-7200 a two-stage light-gas gun. These conditions are achieved by impact of projectiles accelerated to This project produces novel materials (crystal velocities up to 8 km/s. Shock temperatures up to structures, microstructures, and properties) using high 5000 K at 1 Mbar were measured by a fast optical shock pressures. The terms dynamic and shock are spectrometer and show that hydrogen undergoes a used synonymously in this context. Tuneable shock continuous dissociative phase transition above pressure pulses are produced by the impact of a 200 kbar. This continuous dissociation absorbs energy, projectile launched from a small two-stage light-gas which causes lower temperatures and higher densities gun. Shock pressures range from 0.01-1 Mbar, in the Mbar shock pressure range than was thought temperatures range from 50 up to a few 1000°C, strain previously. rates on loading range above 108/s and quench rates on release of pressure are 1012 bar/s and 109 K/s in Electrical conductivities were measured using metal specimens which are recovered intact for investigation. electrodes at pressures in the range 1 to 2 Mbar at A gas gun is used to achieve these high shock calculated temperatures of 2000 to 4000 K. A novel pressures. Specimens range from 1 micron to 3 mm technique was used to produce just enough shock thick and from 3 to 23 mm in diameter. The observed heating to excite just enough electronic carriers to be material structures are correlated with computational able to measure the electrical conductivity of hydrogen simulations to enhance understanding of the effects at Mbar pressures in the short time duration of the produced. For example, a computational model of the experiment. These are the only electrical conductivity dynamic compaction of nanocrystalline Al particles was measurements on condensed hydrogen at any shown to be in good agreement with the structure of pressure. This project, for the first time, metallized compacts produced experimentally. A wide variety of hydrogen at 1.4 Mbar and 3000 K in the fluid and materials characterization measurements are made determined the density dependence of the electronic both before and after 3polication of high dynamic bandgap in the molecular fluid phase. The observed pressures, including X-ray uiiluction, TEM, SEM, metallization pressure in the fluid is about one-half what magnetization, NMR, ana neutron scattering. Over the was predicted for the solid at 0 K. past few years nanocrystalline Al, ceramic, and magnetic powders have been dynamically compacted, Keywords: Shock Pressures, Shock Temperatures, unusual glass has been produced in bulk and Electrical Conductivities, Gas Gun, nanocrystalline Si in grain boundaries by shock com- Hydrogen, Cryogenics, Equation of State, pressing quartz single crystals, and impacts in nature Dissociation, Metallization have been investigated by studying structural effects in shocked minerals. A new gas breach to achieve shock 372. ATOMIC LEVEL EXPLOSIVE CALCULATIONS pressures of <50 Kbar to induce high densities of $400,000 defects and compact powders was built in FY 1997. DOE Contact: Maurice Katz, (202) 586-5799 LLNL Contacts: Larry Fried, (925) 422-7796 Keywords: Shock Pressures, Gas Gun, Materials Characterization, Ceramics, Magnets, A package of atomic-level calculations has been Nanocrystalline Si, Glass assembled that will allow design of new explosive molecules. The package includes calculations of solid density, heat of formation, chemical stability and

170 Office of Fossil Energy

sensitivity. This package is being tried on various new 374. AFM INVESTIGATIONS OF CRYSTAL GROWTH postulated compositions in concert with feedback from $290,000 three organic and inorganic synthesis chemists. The DOE Contact: G. J. D'Alessio, (301) 903-6688 intent is to couple Molecular Design with actual LLNL Contact: J. J. DeYoreo, (925) 423-4240 synthesis routes at the start so that the final selected design will be something with a good chance of being The nanometer-scale morphology of crystalline surfaces made in the lab. The target is to provide 10 to exerts a strong control on materials properties and 15 percent more detonation energy than CL-20 with no performance. While many researchers have studied decrease in sensitivity, vapor deposited metal and semiconductor surfaces grown far from equilibrium, few studies have given Keywords: Energetic Materials, High Explosives, attention to the morphology of crystal surfaces grown Molecular Design, Detonation from melts or solutions near equilibrium despite the fact that most bulk crystals are grown in this regime. 373. METASTABLE SOLID-PHASE HIGH ENERGY Understanding the mechanisms of growth and the origin DENSITY MATERIALS of defects in such crystals can impact materials $535,000 performance in a number of fields including optics, DOE Contact: Maurice Katz, (202) 586-5799 electronics, molecular biology, and structural biology. LLNL Contacts: H. Lorenzana, We are using atomic force microscopy (AFM) to (925) 422-8982 and M. Finger, investigate the growth of single crystal surfaces from (925) 422-6370 solution in order to determine the mechanism of growth, the kinetics of step advancement, the effect of Conventional energetic materials such as propellants, impurities, and the origin of defects. explosives and fuel cells store energy within internal bonds of molecules. This work is exploring the predicted This method has been applied to inorganic, organic and existence of novel materials that are calculated to store macromolecular crystals each of which serve as two to four times the energy content per volume of important model systems. These include KH2PO4, existing explosives, a dramatic improvement in CaCO 3 doped with amino acids, molecular tapes of performance. Though the atomic components are diketopipeizine derivatives, the protein canavalin and similar to standard energetic materials, these new the satellite tobacco mosaic virus. The results of these materials differ from conventional molecular systems in investigations are providing an understanding of the that they form infinite, three-dimensional networks of fundamental physical controls during solvent mediated covalent bonds, otherwise known as extended" solids. crystallization. Every bond in these new systems is energetic; the result is a correspondingly larger storage of energy per Keywords: Morphology, Crystal Surfaces, Atomic Force volume. Specifically, pure nitrogen is calculated to be Microscopy recoverable at ambient conditions as an energetic solid with three times the energy content of HMX, a very high 375. URANIUM CASTING PROGRAM performance explosive. Since these materials are $1,000,000 predicted to exist at high pressures and high DOE Contact: Marshall Sluyter, (301) 903-5491 temperatures, experimental capabilities have been LLNL Contact: Jeff Kass, (925) 422-4831 developed for synthesizing and characterizing such compounds at megabar pressures. The uranium casting program is addressing the use of permanent molds for near net shape castings, The existence of a new extended solid (polymeric) controlled cooling for segregation and microstructure phase of CO has been verified at about 50 kbar. This control and the effect of alloy additions and subsequent new material is recoverable at ambient conditions, and heat treatment on microstructure. Process modeling has is believed to be energetic. The equation-of-state of played a key role in producing high quality castings in various candidate structures for CO have been uranium and uranium alloys. calculated, but further experimental constraints are needed in the structure and bond nature. Accordingly, Keywords: Uranium Casting Raman measurements of absorption in the visible and infrared have been performed. This information has 376. URANIUM SPIN FORMING provided important insights as to the character of the $1,500,000 bonds present in this material. During FY 1997 DOE Contact: Marshall Sluyter, (301) 903-5491 techniques for generating 'large' samples of the LLNL Contact: Jeff Kass, (925) 422-4831 extended-solid phase of CO at high pressures have been developed, in order to measure stoichiometry and Spin forming is being explored as a method to produce energy content. near net shape wrought uranium components. Process Keywords: Energetic Materials, High Energy Density Materials

171 Office of Fossil Energy

modeling has been useful in predicting stress/ strain 200 pm polyimide ablator coating on a 2 mm diameter distribution and spring back. Near net shape compo- capsule target for the National Ignition Facility (NIF). nents have been produced. Such targets should be strong enough to hold the full DT fuel load (about 300 atm) at room temperature, Keywords: Spin Forming allowing us important flexibility in fielding these capsules for ignition experiments. 377. PLUTONIUM NEAR NET SHAPE CASTING $2,500,000 Keywords: Polymers, Laser Fusion Targets, Polyimide, DOE Contact: Marshall Sluyter, Ablator (301) 903-5491 LLNL Contact: Jeff Kass, (925) 422-4831 381. BERYLLIUM ABLATOR COATINGS FOR NIF TARGETS Near net shape casting is being explored using $600,000 permanent molds. High quality castings have been DOE Contact: G. J. D'Alessio, (301) 903-6688 produced. Process modeling has played a significant LLNL Contacts: R. McEachem, (925) 423-4734, role in defining conditions needed for solidification R. Cook, (925) 422-3117, R. Wallace, control. (925) 423-7864 and A. Jankowski, (925)423-2519 Keywords: Shape Casting This program has as its objective the development of 378. ELECTRON BEAM COLD HEARTH MELTING sputter deposition techniques that will allow us to OF URANIUM deposit 150 to 200 pm of a strong, smooth, Cu-doped $900,000 Be ablator on a spherical plastic mandrel shell. These DOE Contact: Marshall Sluyter, (301) 903-5491 Be coated capsule targets have been shown by LLNL Contact: Jeff Kass, (925) 422-4831 calculation to offer some important advantages as ignition targets for the National Ignition Facility (NIF). An existing electron beam evaporation chamber has been modified to produce controlled solidification Keywords: Beryllium, Laser Fusion Targets, Ablator, uranium alloy ingots. Scrap feeders of various types are Sputter Deposition being evaluated. High quality ingots which meet the applicable uranium alloy specification have been produced. ....:R:RY|OS|IALAMOSNATONAL, O Keywords: Electron Beam Melting, Uranium MATERIALS PREPARATION, SYNTHESIS, 379. NIF CAPSULE MANDREL R&D DEPOSITION, GROWTH OR FORMING $800,000 DOE Contact: G. J. D'Alessio, (301) 903-6688 382. RAPID SOLIDIFICATION PROCESSING LLNL Contact: R. Cook, (925) 422-3117 $500,000 DOE Contact: R. Jones, (301) 903-6688 This program has as its objective the development of LANL Contact: D.J. Thoma, (505) 665-3645 2 mm thin-walled plastic shells that will serve as the mandrel for the production of capsule targets for the The project incorporates process development and National Ignition Facility (NIF). The mandrels must be product comparisons resulting from rapid solidification extremely spherical (<1 pm out of round), have wall processing techniques including melt spinning and gas thickness uniformity better than 1 pm, and have a atomization. Alloy homogeneity, phase stability, surface finish of less than 10 nm (rms over modes >9). mechanical and physical properties are used for Several routes are being explored, comparison.

Keywords: Polymers, Laser Fusion Targets, Keywords: Rapid Solidification, Melt Spinning, Microencapsulation, Microshells Atomization, Phase Stability, Alloy Homogeneity 380. POLYIMIDE COATING TECHNOLOGY FOR ICF TARGETS 383. STRUCTURAL ALLOY DEVELOPMENT $500,000 $2,000,000 DOE Contact: G. J. D'Alessio, (301) 903-6688 DOE Contact: Yok Chen, (301) 903-4174 LLNL Contacts: R. Cook, (925) 422-3117 and LANL Contact: D.M. Parkin, (505) 6678455 Steve Letts, (925) 422-4373 Alloy development for high temperature applications This program has as its objective the development of a has focused on laves phase and silicide-based vapor based, high strength polyimide coating tech- materials. Synthesis incorporates rapid solidification, nology that will allow us to produce a smooth, 150 to plasma arc melting, vacuum arc melting, and powder

172 Office of Fossil Energy synthesis techniques. Characterization is performed to techniques. Neutron resonance Doppler broadening detail phase stability and transformation experiments are being performed to understand the thermodynamics, microstructure evolution, mechanical phonon behavior of Pu alloys and phonon densities of properties and high-temperature oxidation. states (PDOS) measurements will be made across the phase boundaries of Pu. The ability to measure Keywords: Laves Phase, Silicide, Rapid Solidification, crystallographic texture in plutonium has been Plasma Arc Melting, Vacuum Arc Melting, demonstrate. The intent is to correlate texture Powder Synthesis measurements with elastic properties.

MATERIALS STRUCTURE OR COMPOSITION Keywords: Neutron Scattering, Pair-distribution- function, Phonon Densities, High Explosives, 384. NATIONAL HIGH MAGNETIC FIELD Plutonium, Uranium, Beryllium and Organic LABORATORY Salts $1,800,000 DOE Contact: J.J. Smith, (301) 903-4269 MATERIALS PROPERTIES, BEHAVIOR, LANL Contact: D.M. Parkin, (505) 667-8455 CHARACTERIZATION OR TESTING

The objective of the thrust is to apply high magnetic 386. DYNAMIC MECHANICAL PROPERTIES OF fields to the solution of unresolved fundamental WEAPONS MATERIALS problems in many body physics of condensed matter. $2,000,000 Particular attention is given to electronic structure and DOE Contact: B.B. Agrawal, (301) 903-2057 many-body phenomena in 5f systems, with special LANL Contact: G.T. Gray III, (505) 667-5452 emphasis on plutonium. There are two major components of the thrust: (1) an examination of static or This program is focused on experimental mean-field properties of correlated-electron systems measurements and computer modeling of dynamic and (2) an examination of rapid femtosecond dynamics stress-strain and fracture behavior of polymers, high of electron-electron correlations (many-body explosives, actinides, beryllium, and common structural phenomena) in high magnetic fields. materials. Development of constitutive relationships and fracture models for the prediction of material The world's longest-pulse, high-field magnet, funded by performance. DOE, will be collocated with the other components of the Los Alamos NHMFL Pulsed-Field Facility, funded by Keywords: Dynamic Properties, Fracture, Microstructure the National Science Foundation (NSF). This interagency DOE/NSF collaboration will provide a 387. DEFORMATION CHARACTERIZATION AND unique user facility to users from DOE laboratories, MODELING industry, and universities. The magnet, when completed $5,000,000 in 2000, will provide nondestructive 100-tesla magnetic DOE Contact: Yok Chen, (301) 903-4174 fields for periods lasting up to 10 milliseconds, which is LANL Contact: D.M. Parkin, (505) 667-8455 a thousand times longer than is available anywhere else. The magnet is a uniquely powerful tool for This program is focused on experimental measure- studying high-temperature superconductors and the ments and computer modeling of elastic-plastic electronic structure of materials at unprecedented deformation paths incorporating dislocation dynamic resolution. and crystallographic texture to define multi-dimensional yield surfaces. Program success will result in an Keywords: High Magnetic Fields, Electronic Structure, improved understanding of materials properties Electron-electron Correlations, Plutonium incorporating theories and modeling to extrapolate from microscopic to mesoscopic properties of materials. 385. NEUTRON DIFFRACTION $1,500,000 Keywords: Elastic-Plastic Deformation, Dislocations, DOE Contact: B.B.Agrawal, (301) 903-2057 Crystallographic Texture LANL Contact: E.M.Farnum, (505) 665-5523 388. MATERIALS AGING Neutron scattering is being applied to the $11,000,000 characterization of weapons materials in the realms of DOE Contact: D.V. Feather, (301) 903-5815 electronic structure, crystallography, chemical reaction LANL Contact: L. Salazar, (505) 667-7485 dynamics and residual strain distribution. The primary materials of interest are high explosives, plutonium, The materials aging program is developing tools, uranium, beryllium and organic salts. techniques, and procedures to advance our capability to measure, analyze, and predict the aging of materials The local structure of Pu and its alloys is being studied within nuclear weapons. Experimental work is using neutron pair-distribution-function (PDF) proceeding in high explosives, polymers, plutonium,

173 Office of Fossil Energy uranium, salts, and beryllium. Experimental 391. ADVANCED ENGINEERING METHODS investigations are proceeding at the atomistic level to DEVELOPMENT examine radiolytic-induced structural changes, $1,100,000 molecular levels for polymer degradation, DOE Contact: R. Jones (301) 903-6688 microstructure and bulk levels for mechanical property LANL Contact: C.A. Spirio, (505) 667-4772 changes or corrosion. The project is focused on developing tools and methods Keywords: High Explosives, Polymers, Plutonium, to support a models-based engineering-manufacturing Uranium, Salts, Beryllium, Atomistic (MBE-M) approach (solid models, assembly animation, Bonding, Molecular Dynamics, Mechanical spline algorithms, sensitivity analysis of secondaries, Properties, Corrosion and manufacturing applications) to both the above ground experimental program, and as-built or 389. POWDER CHARACTERIZATION remanufactured stockpile systems. $300,000 DOE Contact: BIB. Agrawal, (301) 903-2057 Keywords: Solid Model, Spline, Model-based LANL Contact: J.K. Bremser, (505) 667-1179 Engineering, As-built, Remanufacturing, Stockpile Synthesis and processing of ceramic or metal powders depends critically on the physical characterization of the 392. COMPONENT FABRICATION starting powders being used. Typical starting powders $10,000,000 include commercial powders of thoria, magnesia, DOE Contact: R. Jones (301) 903-6688 alumina, tungsten, copper, tungsten carbide, and boron LANL Contact: R. Mah, (505) 667-3238 carbide. In the past year, considerable effort has been expended on characterizing palladium alloy powders. Component fabrication includes the development and Physical properties of interest include particle size and modeling of process technologies coupled with distribution, surface area, bulk and packed densities, extensive materials characterization for the manufacture morphology, pore size and distribution, and zeta of demonstration and test components. Processing potential. The crystalline-phase composition of the capabilities cover casting, forming, atomization, rapid starting powders and processed powders can be solidification processing, powder consolidation, plasma determined by X-ray diffraction, spray, heat treatment, sintering, welding and joining. Characterization includes X-ray diffraction, microscopy, Keywords: Ceramic Powder, Metal Powder, Particle mechanical properties and physical properties Size, Superconducting Powder, X-ray determinations. Materials fabricated include uranium, Diffraction, Surface Area beryllium, stainless steels, refractory metals, palladium, and special alloys. DEVICE OR COMPONENT FABRICATION, BEHAVIOR OR TESTING Keywords: Casting, Forming, Atomization, Rapid Solidification Processing, Powder 390. MANUFACTURING PROCESS DEVELOPMENT Consolidation, Plasma Spray, Heat $8,000,000 Treatment, Sintering, Welding, Joining, DOE Contact: G.S. Hearron, (505) 845-5311 X-ray Diffraction, Microscopy, Mechanical LANL Contact: T.R. Neal, (505) 665-5568 Properties, Physical Properties, Uranium, Beryllium, Stainless Steels, Refractory The Advanced Design and Process Technology Metals, Palladium, Special Alloys program, ADAPT, has taken the role of catalyst for manufacturing-related goals and for integrating the 393. LASER TARGET FABRICATION weapons complex manufacturing activities. This $5,000,000 program includes the development of manufacturing DOE Contact: C. Keane, (301) 903-4323 process improvements, agile manufacturing techniques, LANL Contact: L.R. Foreman, (505) 667-1846 enterprise integration focusing on material resource modeling, and hedge planning for the rapid The fabrication of complex and ultra-precision targets, reconstitution of large-scale production. Investments in mm-sized, for laser drive experiments related to inertial the later three categories have been modest because of confinement fusion and nuclear weapons research. the intensity of needs in process development. ADAPT Efforts include the development and characterization of is directly integrated with core R&D for specific studies special alloys and tritium loading techniques along with of materials performance, models-based engineering, the application of manufacturing processes of rapid and manufacturing specifications. solidification, powder consolidation, physical vapor deposition, chemical vapor deposition, polymer and Keywords: Radioactive Materials, Plutonium Alloys, polymer foam synthesis, precision machining and Beryllium, Uranium, Lithium Salts, Polymers, micro-assembly. Characterization includes High Explosives, Tritium, Welding, Forming, examinations of microstructure, mechanical properties, Casting, Uranium Purification physical properties, nondestructive examinations

174 Office of Fossil Energy

(radiography and ultrasonic), dimensional inspection, and optical interferometry.

Keywords: Physical Vapor Deposition, Chemical Vapor Deposition, Polymer Chemistry, Polymer Foam Synthesis, Precision Machining, Micro-assembly, Beryllium, Tritium, Plastics

394. PULSED POWER TARGET FABRICATION $3,000,000 DOE Contact: C. Keane, (301) 903-4323 LANL Contact: W.E. Anderson, (505) 665-3981

Fabrication and characterization of precision liners for high explosive or capacitive discharge pulsed power experiments. Technologies employed include ingot metallurgy processing, physical deposition of coatings, precision machining and micro-assembly. Characteri- zation techniques include microscopy, mechanical properties, nondestructive examinations (radiography and ultrasonic), dimensional inspection, and optical interferometry.

Keywords: Aluminum, Platinum, Gold, Physical Deposition of Coatings, Precision Machining and Micro-assembly

395. ADVANCED STRATEGIC COMPUTING INITIATIVE MATERIALS MODELING $2,000,000 DOE Contact: G.G. Weigand, (202) 586-0568 LANL Contact: R.A. LeSar, (505) 665-0420 The development and bench-marking of advanced computer codes for the prediction of materials performance or processing technology influences on product quality. Models are being developed utilizing a full-three-dimensional first-principles approach to explore sensitivities to performance or processing variables. This includes the demonstration and baseline of engineering analysis codes to predict the engineering performance and reliability margin of the nuclear explosives package to satisfy its stockpile to target sequence requirements.

Keywords: Modeling, Constitutive Relationships, Fracture, Casting, Reliability Margin, Nuclear Explosives Package

175 Office of Fossil Energy

OFFICE OF FOSSIL ENERGY FY 1997

Office of Fossil Enervy - Grand Total $4,914,000

Office of Advanced Research $4,914,000 Fossil Energy AR&TD Materials Program $4,914,000

Materials Preparation. Synthesis. Deposition. Growth or Forming $1,905,000

Coating Process Development for Cr-Nb Alloys 20,000 Procurement of Advanced Austenitic and Aluminide Alloys 50,000 Development of Iron Aluminides 105,000 Development of Cr-Nb Alloys 105,000 High-Strength Iron Aluminide Alloys PYF' Low-Aluminum Content Iron-Aluminum Alloys 54,000 Mo-Si Alloy Development 47,000 Development of Improved and Corrosion Resistant Surfaces for Fossil Power System Components 35,000 Commercial-Scale Melting and Processing of Low-Aluminum Content Alloys PYF1 Development of a Modified 310 Stainless Steel 84,000 Application of Advanced Austenitic Alloys to Fossil Power System Components 135,000 Development of Recuperator Materials 51,000 Influence of Processing on Microstructure and Properties of Aluminides 175,000 Investigation of Electrospark-Deposited Coatings for Protection of Materials in Sulfidizing Atmospheres 100,000 Technology Transfer of Electrospark-Deposited Coatings for Protection of Materials in Sulfidizing Atmospheres 50,000 Fabrication of Fiber-Reinforced Composites by Chemical Vapor Infiltration and Deposition 150,000 Compliant Oxide Coating Development 100,000 Development of Oxidation/Corrosion-Resistant Composite Materials and Interfaces 150,000 Optimization of the Chemical Vapor Infiltration Technique for Ceramic Composites PYF' Transport Properties of Ceramic Composites 50,000 Modeling of Fibrous Preforms for CVD Infiltration 50,000 Corrosion Protection of SiC-Based Ceramics with CVD Mullite Coatings 30,000 Feasibility of Synthesizing Oxide Films on Ceramic and Metal Substrates 44,000 Ceramic Coating and Native Oxide Scales Evaluation 70,000 Carbon Fiber Composite Molecular Sieves 150,000 Activation of Carbon Fiber Composite Molecular Sieves PYF' Carbon Fiber Composite Molecular Sieves Technology Transfer 100,000

Materials Properties. Behavior. Characterization or Testing $1,202,000

Investigation of the Weldability of Polycrystalline Iron Aluminides .40,000 Friction Welding of Iron Aluminides 20,000 Evaluation of the Intrinsic and Extrinsic Fracture Behavior of Iron Aluminides 44,000 Investigation of Iron Aluminide Weld Overlays 6,000 Fireside Corrosion Tests of Candidate Advanced Austenitic Alloys, Coatings, and Claddings 33,000

'PYF denotes that funding for this project, active in FY 1997, was provided from prior year allocations.

176 Office of Fossil Energy

OFFICE OF FOSSIL ENERGY (continued) FY 1997

Office of Advanced Research (continued)

Fossil Eneray AR&TD Materials Program (continued)

Materials Properties. Behavior. Characterization or Testing (continued)

Joining Techniques for Advanced Austenitic Alloys PYF' Fatigue and Fracture Behavior of Cr-Nb Alloys 35,000 Corrosion and Mechanical Properties of Alloys in FBC and Mixed-Gas Environments 180,000 High Temperature Environmental Effects on Iron Aluminides 170,000 Investigation of Moisture-Induced Embrittlement of Iron Aluminides 9,000 Reduction of Defect Content in ODS Aloys 30,000 Corrosion Protection of Ultrahigh Temperature Intermetallic Alloys 130,000 Oxide Dispersion Strengthened (ODS) Iron Aluminides 295,000 Materials Support for HITAF PYF' Support Services for Ceramic Fiber-Ceramic Matrix Composites 30,000 Development of Nondestructive Evaluation Methods and Effects of Flaws on the Fracture Behavior of Structural Ceramics 180,000 Device or Component Fabrication. Behavior or Testing $1,361,000

Materials and Components in Fossil Energy Applications Newsletter 50,000 Development of Ceramic Membranes for Gas Separation and Fuel Cells 450,000 Extrusion Press Equipment 75,000 High-Temperature Heat Exchanger and Hot-Gas Filter Development PYF' Investigation of the Mechanical Properties and Performance of Ceramic Composite Components PYF' Solid State Electrolyte Systems 553,000 Oxide-Dispersion-Strengthened Fe3AI-Based Alloy Tubes 33,000 ODS Fe3AI Tubes for High-Temperature Heat Exchangers 50,000 Iron Aluminide Filters for IGCCs PYF' Iron Aluminide Filters for PFBCs 50,000 Ceramic Tubesheet Design Analysis PYF' Dense Ceramic Tube Development 100,000

Instrumentation and Facilities $ 446,000 Management of the Fossil Energy AR&TD Materials Program 406,000 General Technology Transfer Activities 35,000 Gordon Research Conference Support 5,000

'PYF denotes that funding for this project, active in FY 1997, was provided from prior year allocations.

177 Office of Fossil Energy

OFFICE OF FOSSIL ENERGY

The Office of Fossil Energy responsibilities include management of the Department's fossil fuels (coal, oil and natural gas) research and development program. This research is generally directed by the Office of Coal Technology (OCT), the Office of Gas and Petroleum Technology, and the Office of Advanced Research and Special Technologies in support of the National Energy Strategy Goals for Increasing Energy Efficiency, Securing Future Energy Supplies, Respecting the Environment, and Fortifying our Foundations. Three specific fossil energy goals are currently being pursued:

1. The first is to secure liquids supply and substitution. This goal targets the enhanced production of domestic petroleum and natural gas, the development of advanced, cost-competitive alternative fuels technology, and the development of coal-based, end-use technology to substitute for oil in applications traditionally fueled by liquid and gaseous fuel forms. 2. The second is to develop power generation options with environmentally superior, high-efficiency technologies for the utility, industrial, and commercial sectors. This goal targets the development of super-clean, high-efficiency power generation technologies.

3. The third is to pursue a global technology strategy to support the increased competitiveness of the U.S. in fossil fuel technologies, to maintain world leadership in our fossil fuel technology base, and provide expanded markets for U.S. fuels and technology. This crosscutting goal is supported by the activities in the above two technology goals.

OFFICE OF ADVANCED RESEARCH MATERIALS PREPARATION, SYNTHESIS, DEPOSITION, GROWTH OR FORMING FOSSIL ENERGY AR&TD MATERIALS PROGRAM 396. COATING PROCESS DEVELOPMENT FOR Fossil Energy (FE) materials-related research is con- Cr-Nb ALLOYS ducted under an Advanced Research and Technology $20,000 Development (AR&TD) Materials sub-activity and is an DOE Contacts: F. M. Glaser, (301) 903-2784 and integral part of the R&D conducted by the Office of M. H. Rawlins, (423) 576-4507 Advanced Research and Special Technologies. The Oak Ridge National Laboratory Contact: AR&TD Materials program includes cross-cutting R. R. Judkins, (423) 574-4572 research to obtain a fundamental understanding of Ohio State University Contact: R. A. Rapp, materials and how they perform in fossil-based process (614) 292-6178 environments and the development of new classes of generic materials that will allow the development of new Cr-Nb alloys are being developed for high temperature fossil energy systems or major improvements in existing service, but require protection from high temperature systems. The present program is focused on ceramics environments, such as oxidation. Previously developed (composite structural ceramics, catalyst supports, solid MoSi 2-base coatings have shown some promise for pro- state electrolytes, membranes, and ceramic filters), new tecting Nb, and the principles learned may have applica- alloys (aluminides, filters, advanced austenitic steels, bility for protective coatings of Cr-Nb. The purpose of and coatings and claddings), corrosion research, and this work is to examine the protection of Cr-Nb alloys technology development and transfer. with either silicides or aluminides.

The AR&TD research is carried through development Keywords: Alloys, Aluminizing, Chromizing, Corrosion, and technology transfer to industry. Special emphasis is Coatings given to technology transfer to ensure that the materials will be available for subsequent fossil commercial 397. PROCUREMENT OF ADVANCED AUSTENITIC applications. This also enhances U.S. technological AND ALUMINIDE ALLOYS competitiveness not only in the fossil area but in the $50,000 materials industry in general and other technology DOE Contacts: F. M. Glaser, (301) 903-2784 and application areas as well. The research is conducted in M. H. Rawlins, (423) 576-4507 industry, universities, not-for-profit agencies, and Oak Ridge National Laboratory Contact: national laboratories. This widespread participation also R. R. Judkins, (423) 574-4572 helps maintain the U.S. materials technology capabilities. This task provides funds for the procurement of alloys necessary for alloy development and testing activities of the AR&TD Materials Program.

Keywords: Alloys, Aluminides, Austenitic

178 Office of Fossil Energy

398. DEVELOPMENT OF IRON ALUMINIDES as structural components of advanced fossil energy $105,000 conversion systems. DOE Contacts: F. M. Glaser, (301) 903-2784 and M. H. Rawlins, (423) 576-4507 Keywords: Alloys, Aluminides, Microalloy Oak Ridge National Laboratory Contact: G. M. Goodwin, (423) 574-4809 401. LOW-ALUMINUM CONTENT IRON-ALUMINUM ALLOYS The objective of this task is to develop low-cost and $54,000 low-density intermetallic alloys based on Fe3AI with an DOE Contacts: F. M. Glaser, (301) 903-2784 and optimum combination of strength, ductility, weldability, M. H. Rawlins, (423) 576-4507 and corrosion resistance for use as components in Oak Ridge National Laboratory Contact: advanced fossil energy conversion systems. Emphasis V. K. Sikka, (423) 574-5112 is on the development of iron aluminides for heat recovery applications in coal gasification systems. The objective of this task is to develop a conventionally-fabricable low-cost and lower density Keywords: Alloys, Aluminides, Intermetallic Compounds iron-aluminum-based alloy with a good combination of strength, ductility, weldability, and corrosion resistance 399. DEVELOPMENT OF Cr-Nb ALLOYS for use as components in advanced fossil energy $105,000 systems. Initial emphasis is on the development of DOE Contacts: F. M. Glaser, (301) 903-2784 and iron-aluminum alloys for heat-recovery applications in M. H. Rawlins, (423) 576-4507 coal gasification systems. Oak Ridge National Laboratory Contact: C. T Liu, (423) 574-4459 Keywords: Alloys, Iron-Aluminum

The objective of this task is to develop high-strength, 402. Mo-SI ALLOY DEVELOPMENT corrosion-resistant intermetallic alloys for use as hot $47,000 components in advanced fossil energy conversion and DOE Contacts: F. M. Glaser, (301) 903-2784 and power generation systems. The successful development M. H. Rawlins, (423) 576-4507 of these alloys is expected to improve the thermal Oak Ridge National Laboratory Contact: efficiency of fossil energy conversion systems through J. H. Schneibel, (423) 574-4644 increased operating temperatures and to increase the service life of hot components exposed to corrosive The objective of this task is to develop new-generation environments at elevated temperatures (1000°C). The corrosion-resistant Mo-Si alloys for use as hot compo- work is focused on in situ composite alloys based on the nents in advanced fossil energy conversion and power Cr-Cr2Nb system. generation systems. The successful development of Mo-Si alloys is expected to improve the thermal Keywords: Alloys, Chromium-Niobium, Corrosion, efficiency and performance of fossil energy systems Intermetallic Compounds through increased operating temperature and to increase the service life of hot components exposed to 400. HIGH-STRENGTH IRON ALUMINIDE ALLOYS corrosive environments at high temperatures (to $0 - PYF' 1600°C). The initial effort is devoted to Mo5Si3-base DOE Contacts: F. M. Glaser, (301) 903-2784 and alloys containing boron additions. M. H. Rawlins, (423) 576-4507 Oak Ridge National Laboratory Contact: Keywords: Alloys, Molybdenum, Silicon C. G. McKamey, (423) 574-6917 403. DEVELOPMENT OF IMPROVED AND The objective of this task is to use microalloying CORROSION RESISTANT SURFACES FOR techniques to further develop the Fe3AI-based alloys. FOSSIL POWER SYSTEM COMPONENTS Emphasis is on producing a low-cost, low-density, $35,000 precipitation-strengthened Fe3AI-based intermetallic DOE Contacts: F. M. Glaser, (301) 903-2784 and alloy with improved high-temperature creep resistance M. H. Rawlins, (423) 576-4507 while maintaining an optimum combination of room- Oak Ridge National Laboratory Contact: temperature and high-temperature (600-700°C) tensile V. K. Sikka, (423) 574-5112 properties, weldability, and corrosion resistance for use A Cooperative Research and Development Agreement (CRADA) has been established with ABB Combustion Engineering for the development of corrosion-resistant surface protection for fossil power systems.

Keywords: Alloys, Iron-Aluminum, Corrosion, 'PYF denotes that funding for this project, active in Technology Transfer FY 1997, was provided from prior year allocations.

179 Office of Fossil Energy

404. COMMERCIAL-SCALE MELTING AND 407. DEVELOPMENT OF RECUPERATOR PROCESSING OF LOW-ALUMINUM CONTENT MATERIALS ALLOYS $51,000 $0 - PYF' DOE Contacts: F. M. Glaser, (301) 903-2784 and DOE Contacts: F. M. Glaser, (301) 903-2784 and M. H. Rawlins, (423) 576-4507 M. H. Rawlins, (423) 576-4507 Oak Ridge National Laboratory Contact: Oak Ridge National Laboratory Contact: R. W. Swindeman, (423) 574-5108 V. K. Sikka, (423) 574-5112 A Cooperative Research and Development Agreement The purpose of this activity is the preparation and (CRADA) has been signed with Solar Turbines, Inc. to evaluation of castings of low-aluminum content, develop a materials technology for recuperators iron-aluminum alloys. The castings will be prepared in operating at gas inlet temperatures to 730°C. several types of molds including: (1) graphite, (2) sand, and (3) investment. Castings will be prepared primarily Keywords: Alloys, Austenitics, Technology Transfer from the air-induction-melted material. Selected graphite and investment castings will also be prepared 408. INFLUENCE OF PROCESSING ON from the vacuum-induction-melted material. The MICROSTRUCTURE AND PROPERTIES OF graphite and sand castings will be prepared at ORNL ALUMINIDES and will also be procured from the commercial $175,000 foundries. The castings will be evaluated for porosity, DOE Contacts: F. M. Glaser, (301) 903-2784 and grain structure, mechanical properties, and weldability. M. H. Rawlins, (423) 576-4507 The mechanical property evaluation will consist of Oak Ridge National Laboratory Contact: Charpy impact, tensile, and creep testing. I. G. Wright, (423) 574-4451 Idaho National Engineering and Environmental Keywords: Alloys, Iron-Aluminum, Melting, Casting Laboratory Contact: R. N. Wright, (208) 526-6127 405. DEVELOPMENT OF A MODIFIED 310 STAINLESS STEEL The purpose of this program is to determine the $84,000 influence of processing on the properties of alloys based DOE Contacts: F. M. Glaser, (301) 903-2784 and on the intermetallic compound Fe3AI. Thermo- M. H. Rawlins, (423) 576-4507 mechanical processing of these alloys is pursued to Oak Ridge National Laboratory Contact: improve their properties. The response of the R. W. Swindeman, (423) 574-5108 microstructure to elevated temperature deformation and subsequent annealing is characterized in terms of the The purpose of this task is to evaluate structural alloys establishment of equilibrium phases and equilibrium for improved performance of high-temperature degree of long-range order. The role of dislocation and components in advanced combined-cycle and antiphase boundary structures in enhancing ductility of coal-combustion systems. Fe3AI is investigated. The tensile properties are determined at room and elevated temperature and Keywords: Materials, Mechanical Properties, related to the microstructure. Reaction synthesis is Austenitics, Hot-Gas investigated as a novel joining method and as a process to fabricate porous iron aluminides for filter 406. APPLICATION OF ADVANCED AUSTENITIC applications. Oxide dispersion strengthened alloys, ALLOYS TO FOSSIL POWER SYSTEM fabricated by reaction synthesis, are developed for COMPONENTS improved high temperature strength. Compositions of $135,000 the Fe3AI alloys and details of the processing are DOE Contacts: F. M. Glaser, (301) 903-2784 and determined in collaboration with the program at Oak M. H. Rawlins, (423) 576-4507 Ridge National Laboratory (ORNL). Oak Ridge National Laboratory Contact: R. W. Swindeman, (423) 574-5108 Keywords: Aluminides, Processing, Microstructure A Cooperative Research and Development Agreement (CRADA) has been established with ABB Combustion Engineering for the development of advanced austenitic alloys for fossil power systems.

Keywords: Alloys, Austenitics, Technology Transfer

'PYF denotes that funding for this project, active in FY 1997, was provided from prior year allocations.

180 Office of Fossil Energy

409. INVESTIGATION OF ELECTROSPARK- for shortest processing time, greatest density and DEPOSITED COATINGS FOR PROTECTION OF maximum strength. MATERIALS IN SULFIDIZING ATMOSPHERES $100,000 Keywords: Composites, Fiber-Reinforced, Ceramics DOE Contacts: F. M. Glaser, (301) 903-2784 and M. H. Rawlins, (423) 5764507 412. COMPLIANT OXIDE COATING DEVELOPMENT Oak Ridge National Laboratory Contact: $100,000 R. R. Judkins, (423) 574-4572 DOE Contacts: F. M. Glaser, (301) 903-2784 and Pacific Northwest National Laboratory Contact: M. H. Rawlins, (423) 576-4507 R. N. Johnson, (509) 375-6906 Oak Ridge National Laboratory Contact: D. P. Stinton, (423) 574-4556 The purpose of this task is to examine the use of the electrospark deposition coating process for the Monolithic SiC heat exchangers and fiber-reinforced application of corrosion-, erosion-, and wear-resistant SiC-matrix composite heat exchangers and filters are coatings to candidate heat exchanger (including susceptible to corrosion by alkali metals at elevated superheater and reheater) alloys. Materials to be temperatures. Protective coatings are currently being deposited may include MCrAI, MCrAIY, highly developed to isolate the SiC materials from the wear-resistant carbides, and other hardsurfacing corrodents. Unfortunately, these coatings typically crack materials. and spall when applied to SiC substrates. The purpose of this task is to determine the feasibility of using a Keywords: Coatings, Materials, Deposition compliant material between the protective coating and the substrate. The low-modulus compliant layer could 410. TECHNOLOGY TRANSFER OF ELECTRO- absorb stresses and eliminate cracking and spalling of SPARK DEPOSITED COATINGS FOR the protective coatings. PROTECTION OF MATERIALS IN SULFIDIZING ATMOSPHERES Keywords: Ceramics, Oxides, Coatings $50,000 DOE Contacts: F. M. Glaser, (301) 903-2784 and 413. DEVELOPMENT OF M. H. Rawlins, (423) 576-4507 OXIDATION/CORROSION-RESISTANT Oak Ridge National Laboratory Contact: COMPOSITE MATERIALS AND INTERFACES I. G. Wright, (423) 574-4451 $150,000 Pacific Northwest National Laboratory Contact: DOE Contacts: F. M. Glaser, (301) 903-2784 and R. N. Johnson, (509) 375-6906 M. H. Rawlins, (423) 576-4507 Oak Ridge National Laboratory Contact: The purpose of this task is to transfer to industry the R. A. Lowden, (423) 576-2769 electrospark deposition coating process technology for the application of corrosion-, erosion-, and Fiber-reinforced SiC-matrix composites have been wear-resistant coatings to candidate heat exchanger observed to fail in fossil energy applications for two (including superheater and reheater) alloys. reasons. First, the mechanical properties of composites deteriorate under stressed oxidation because oxidants Keywords: Coatings, Materials, Deposition such as steam penetrate cracks formed in the SiC matrix and react with the carbon or boron nitride inter- 411. FABRICATION OF FIBER-REINFORCED face. The mechanical properties of composites may COMPOSITES BY CHEMICAL VAPOR degrade because of corrosion due to sodium species INFILTRATION AND DEPOSITION typically present in fossil systems. Therefore, the $150,000 purposes of this task are to first, develop fiber-matrix DOE Contacts: F. M. Glaser, (301) 903-2784 and interfaces that are resistant to oxidation and yet M. H. Rawlins, (423) 576-4507 optimize the mechanical behavior of composites, and Oak Ridge National Laboratory Contact: second, to develop protective overcoats or oxide T. M. Besmann, (423) 574-6852 matrices that are resistant to oxidation and corrosion.

The purpose of this task is to develop a process for the Keywords: Composites, Ceramics, Fiber-Reinforced, fabrication of fiber-reinforced ceramic composites Interfaces having high fracture toughness and high strength. This process utilizes a steep temperature gradient and a pressure gradient to infiltrate low-density fibrous structures with gases, which deposit solid phases to form the matrix of the composite. Further development of this process is needed to fabricate larger components of more complex geometry, and to optimize infiltration

181 Office of Fossil Energy

414. OPTIMIZATION OF THE CHEMICAL VAPOR 416. MODELING OF FIBROUS PREFORMS FOR INFILTRATION TECHNIQUE FOR CERAMIC CVD INFILTRATION COMPOSITES $50,000 $0 - PYF' DOE Contacts: F. M. Glaser, (301) 903-2784 and DOE Contacts: F. M. Glaser, (301) 903-2784 and M. H. Rawlins, (423) 576-4507 M. H. Rawlins, (423) 576-4507 Oak Ridge National Laboratory Contact: Oak Ridge National Laboratory Contact: D. P. Stinton, (423) 574-4556 D. P. Stinton, (423) 574-4556 Georgia Institute of Technology Contact: University of Tennessee Contact: P. K. Liaw, T L. Starr, (404) 894-0579 (423) 974-6356 The purpose of this project is to conduct a theoretical This project is focused on an optimization of the forced and experimental program to develop an analytical chemical vapor infiltration technique for fabrication of model for the fabrication and infiltration of fibrous ceramic matrix composites (CMCs) using process preforms. The analytical model will: (1) predict preform models. In particular, a process model developed at the structure (density, porosity, fiber orientation, etc.) based Georgia Tech Research Institute shall be thoroughly on fabrication technique and fundamental fiber investigated. Experimental verification of the process parameters (diameter, aspect ratio, etc.), and (2) predict model shall be conducted in light of microstructural permeation and heat conduction through the preform characterization using both destructive and structure and, thus, predict the CVD infiltration nondestructive evaluation techniques. An optimized performance. process for manufacturing CMCs shall be demonstrated. Moreover, mechanistic understanding regarding Keywords: Ceramics, Composites, Modeling the effects of processing parameters on microstructural features, and fatigue and fracture behavior of CMCs 417. CORROSION PROTECTION OF SIC-BASED shall be provided. CERAMICS WITH CVD MULLITE COATINGS $30,000 Keywords: Composites, Fiber-Reinforced, Ceramics DOE Contacts: F. M. Glaser, (301) 903-2784 and M. H. Rawlins, (423) 5764507 415. TRANSPORT PROPERTIES OF CERAMIC Oak Ridge National Laboratory Contact: COMPOSITES D. P. Stinton, (423) 574-4556 $50,000 Boston University Contact: Vinod Sarin, DOE Contacts: F. M. Glaser, (301) 903-2784 and (617) 353-6451 M. H. Rawlins, (423) 576-4507 Oak Ridge National Laboratory Contact: This project involves the growth of dense mullite D. P. Stinton, (423) 574-4556 coatings on SiC-based substrates by chemical vapor Georgia Institute of Technology Contact: deposition. SiC and SiC-based composites have been T. L. Starr, (404) 894-0579 identified as the leading candidate materials for stringent elevated temperature applications. At The purpose of this research effort is to conduct a moderate temperatures and pressures, the formation of theoretical and experimental program to identify new a thin self-healing layer of SiO2 is effective in preventing compositions and processing methods to improve the catastrophic oxidation by minimizing the diffusion of 02 physical and mechanical properties of selected to the substrate. The presence of impurities can fiber-reinforced ceramics. The ceramic matrix material increase the rate of passive oxidation by modifying the is amorphous fused silica or modified silica glass, and transport rate of oxygen through the protective scale, the focus is the development of fiber-reinforced silica. can cause active oxidation via formation of SiO which Parameters studied include: (1) differences in elastic accelerates the degradation process, or can produce modulus between matrix and fiber, (2) differences in compositions such as Na2SO 3 which chemically attack thermal expansion, (3) nature of interfacial bond, the ceramic via rapid corrosion. There is therefore a (4) densification of matrix, (5) nature of fiber critical need to develop adherent oxidation/corrosion- fracture/pull-out, (6) fiber diameter and fiber resistant, and thermal-shock-resistant coatings that can length-to-diameter ratio, (7) fiber loading, and (8) fiber withstand such harsh environments. Mullite has been dispersion and orientation. A model will be developed identified as an excellent candidate material due to its based on the information generated in the experimental desirable properties of toughness, corrosion resistance, phase of the program. and a good coefficient of thermal expansion match with SiC. Keywords: Ceramics, Composites, Fiber-Reinforced Keywords: Ceramics, Coatings

'PYF denotes that funding for this project, active in FY 1997, was provided from prior year allocations.

182 Office of Fossil Energy

418. FEASIBILITY OF SYNTHESIZING OXIDE FILMS 420. CARBON FIBER COMPOSITE MOLECULAR ON CERAMIC AND METAL SUBSTRATES SIEVES $44,000 $150,000 DOE Contacts: F. M. Glaser, (301) 903-2784 and DOE Contacts: F. M. Glaser, (301) 903-2784 and M. H. Rawlins, (423) 576-4507 M. H. Rawlins, (423) 576-4507 Oak Ridge National Laboratory Contact: Oak Ridge National Laboratory Contact: D. P. Stinton, (423) 574-4556 T. D. Burchell, (423) 576-8595 Lawrence Berkeley National Laboratory Contact: lan Brown, (510) 486-4174 Hydrogen recovery technologies are required to allow the upgrading of heavy hydrocarbons to transport fuels, The objective of this project is the study of the feasibility thus reducing the amount of carbon rejected during the of synthesizing metal oxide ceramic films on ceramic conversion of fossil resources into hydrocarbon and metal substrates. This feasibility will be products. The purpose of this work is to develop carbon demonstrated by use of plasma-based deposition and molecular sieves (CMS) starting with porous carbon ion mixing techniques. The films shall be characterized fiber composites (CFC) manufactured from petroleum for properties such as composition, structure, hardness, pitch derived carbon fibers. The carbon fiber composite high temperature oxidation resistance, adhesion to the molecular sieves (CFCMS) will be utilized in pressure substrate, and stability to high temperature cycling. The swing adsorption units for the efficient recovery of value of intermediate transition or buffer layers, hydrogen from synthesis gas, refinery purge gases, and composed of materials with suitably matched thermal for other gas separation operations associated with expansion characteristics and atomically graded hydrogen recovery. interfaces, as a technique for improving the high temperature survivability of the films, shall be explored. Keywords: Carbon Fibers, Sieves, Composites Samples shall be formed on substrates of various shapes and sizes, including perhaps on the inside and 421. ACTIVATION OF CARBON FIBER COMPOSITE outside of pipes, as well as on small flat coupons. The MOLECULAR SIEVES issue of deposition onto and atomic mixing into $0 - PYF1 substrates which are insulating shall be addressed DOE Contacts: F. M. Glaser, (301) 903-2784 and experimentally. The work is divided into two parts: M. H. Rawlins, (423) 576-4507 (1) AI203 films on alumina-forming alloy substrates, and Oak Ridge National Laboratory Contact: (2) oxides on SiC. R. R. Judkins, (423) 574-4572 Keywords: Ceramics, Films, Oxides University of Kentucky Contact: Frank Derbyshire, (606) 257-0305 419. CERAMIC COATING AND NATIVE OXIDE SCALES EVALUATION A novel monolithic adsorbent carbon, manufactured $70,000 from carbon fibers, has been invented jointly by DOE Contacts: F. M. Glaser, (301) 903-2784 and researchers at Oak Ridge National Laboratory (ORNL) M. H. Rawlins, (423) 576-4507 and the University of Kentucky Center for Applied Oak Ridge National Laboratory Contact: Energy Research. The novel material, referred to as a P. F. Tortorelli, (423) 574-5119 carbon-fiber composite molecular sieve (CFCMS) is fabricated at ORNL in the Carbon Materials Technology The purpose of this work is to generate the information Group. The purpose of this activity is to activate needed for the development of improved (slow growing, samples of the CFCMS and to perform subsequent adherent, sound) protective oxide coatings and scales. analyses of the surface area, pore width distributions, The specific objectives are to systematically investigate and micropore volume. Activities are directed toward an the relationships among substrate composition and understanding of the relationships between the surface oxide structure, adherence, soundness, and activation process and the micro- or mesopore structure micromechanical properties, (2) use such information to that develops. predict scale and coating failures, and (3) identify and evaluate compositions and synthesis routes for Keywords: Carbon Fibers, Sieves, Composites producing materials with damage-tolerant scales and coatings.

Keywords: Coatings, Corrosion

'PYF denotes that funding for this project, active in FY 1997, was provided from prior year allocations.

183 Office of Fossil Energy

422. CARBON FIBER COMPOSITE MOLECULAR procedures for making welds, based on ambient SIEVES TECHNOLOGY TRANSFER temperature properties. $100,000 DOE Contacts: F. M. Glaser, (301) 903-2784 and Keywords: Joining, Welding M. H. Rawlins, (423) 576-4507 Oak Ridge National Laboratory Contact: 425. EVALUATION OF THE INTRINSIC AND T. D. Burchell, (423) 576-8595 EXTRINSIC FRACTURE BEHAVIOR OF IRON ALUMINIDES Hydrogen and methane gas recovery technologies are $44,000 required to: (1) allow the upgrading of heavy hydro- DOE Contacts: F. M. Glaser, (301) 903-2784 and carbons to transport fuels, thus reducing the amount of M. H. Rawlins, (423) 576-4507 carbon rejected during crude oil refining and (2) to Oak Ridge National Laboratory Contact: improve the yield and process economics of natural gas I. G. Wright, (423) 5744451 wells. The purpose of this work is to develop carbon West Virginia University Contact: B. R. Cooper, fiber composite molecular sieves (CFCMS) from porous (304) 293-3423 carbon fiber composites manufactured from solvent extracted coal tar pitch derived carbon fibers. The work The purpose of this activity is the evaluation of the will be performed in collaboration with other members of intrinsic and extrinsic fracture behavior of iron the Cooperative Research Partnership on Carbon aluminides and the study of atomistic simulations of Products and the Non Fuel Uses of Coal. defect concentrations, dislocation mobility, and solute effects in Fe3AI. The work also involves an experimental Keywords: Consortium, Carbon Products study of environmentally-assisted crack growth of Fe3AI at room and at elevated temperatures. The combined MATERIALS PROPERTIES, BEHAVIOR, modeling and experimental activities are expected to CHARACTERIZATION OR TESTING elucidate the mechanisms controlling deformation and fracture in Fe3AI in various environments. 423. INVESTIGATION OF THE WELDABILITY OF POLYCRYSTALLINE IRON ALUMINIDES Keywords: Alloys, Aluminides, Fracture $40,000 DOE Contacts: F. M. Glaser, (301) 903-2784 and 426. INVESTIGATION OF IRON ALUMINIDE WELD M. H. Rawlins, (423) 576-4507 OVERLAYS Oak Ridge National Laboratory Contact: $6,000 R. W. Swindeman, (423) 574-5108 DOE Contacts: F. M. Glaser, (301) 903-2784 and Colorado School of Mines Contact: M. H. Rawlins, (423) 576-4507 G. R. Edwards, (303) 273-3773 Oak Ridge National Laboratory Contact: R. W. Swindeman, (423) 574-5108 The purpose of this project is the investigation of the Lehigh University Contact: J. N. DuPont, weldability of polycrystalline aluminides. The major (610) 758-3942 thrust of the project is to determine the role of microstructure in the intergranular cracking of aluminides, The objective of this activity is the investigation of iron with special emphasis on weld cracking susceptibility. aluminide weld overlays. Specific tasks include: (1) filler The weldability of polycrystalline Fe3AI-X alloys is being wire development, (2) weldability, (3) oxidation and evaluated, and the weldability is correlated with sulfidation studies, (4) erosion studies, (5) erosion- composition, phase equilibria, grain size and corrosion studies, and (6) field exposures. morphology, domain size, and degree of long-range order. Keywords: Alloys, Aluminides, Overlay, Welding, Joining Keywords: Joining, Welding 427. FIRESIDE CORROSION TESTS OF CANDIDATE 424. FRICTION WELDING OF IRON ALUMINIDES ADVANCED AUSTENITIC ALLOYS, COATINGS, $20,000 AND CLADDINGS DOE Contacts: F. M. Glaser, (301) 903-2784 and $33,000 M. H. Rawlins, (423) 576-4507 DOE Contacts: F. M. Glaser, (301) 903-2784 and Oak Ridge National Laboratory Contact: M. H. Rawlins, (423) 576-4507 I. G. Wright, (423) 574-4451 Oak Ridge National Laboratory Contact: The Welding Institute Contact: P. L. Threadgill, R. W. Swindeman, (423) 574-5108 8-0-11-44-1223-891162 Foster Wheeler Development Corporation Contact: J. L. Blough, (201) 535-2355 The purpose of this project is to establish that friction welding is a feasible method for joining iron aluminide The purpose of this project is to provide comprehensive tubes to other iron aluminide tubes, and to austenitic corrosion data for selected advanced austenitic tube alloys. A companion objective is to establish optimized alloys in simulated coal ash environments. ORNL-

184 Office of Fossil Energy

modified alloys and standard comparison alloys have The microstructure of the alloys shall be characterized been examined. The variables affecting coal ash and correlated with the mechanical properties. corrosion and the mechanisms governing oxide breakdown and corrosion penetration are being evaluated. Keywords: Fracture, Fatigue, Alloys Corrosion rates of the test alloys are determined as functions of temperature, ash composition, gas 430. CORROSION AND MECHANICAL PROPERTIES composition, and time. OF ALLOYS IN FBC AND MIXED-GAS ENVIRONMENTS Keywords: Austenitics, Alloys, Corrosion $180,000 DOE Contacts: F. M. Glaser, (301) 903-2784 and 428. JOINING TECHNIQUES FOR ADVANCED M. H. Rawlins, (423) 576-4507 AUSTENITIC ALLOYS Oak Ridge National Laboratory Contact: $0 - PYF1 I. G. Wright, (423) 574-4451 DOE Contacts: F. M. Glaser, (301) 903-2784 and Argonne National Laboratory Contact: K. Natesan, M. H. Rawlins, (423) 576-4507 (708) 252-5103 Oak Ridge National Laboratory Contact: R. W. Swindeman, (423) 574-5108 The purposes of this task are to: (1) evaluate the University of Tennessee Contact: C. D. Lundin, corrosion mechanisms for chromia- and alumina- (423) 974-5310 forming alloys in mixed-gas environments, (2) develop an understanding of the role of several microalloy Weldability is an important consideration in the constituents in the oxidation/sulfidation process, selection of a suitable alloy for the fabrication of boiler (3) evaluate transport kinetics in oxide scales as components such as superheaters and reheaters. It is functions of temperature and time, (4) characterize often a challenge to select joining materials and surface scales that are resistant to sulfidation attack, establish procedures that will allow advanced materials and (5) evaluate the role of deposits in corrosion to function at their full potential. The purpose of this processes. research is to examine important aspects of newly developed austenitic tubing alloys intended for service Keywords: Corrosion, Gasification, Creep Rupture, in the temperature range 550-700°C. Fluidized-Bed Combustion

Keywords: Alloys, Austenitics, Joining, Welding 431. HIGH-TEMPERATURE ENVIRONMENTAL EFFECTS ON IRON ALUMINIDES 429. FATIGUE AND FRACTURE BEHAVIOR OF $170,000 Cr-Nb ALLOYS DOE Contacts: F. M. Glaser, (301) 903-2784 and $35,000 M. H. Rawlins, (423) 576-4507 DOE Contacts: F. M. Glaser, (301) 903-2784 and Oak Ridge National Laboratory Contact: M. H. Rawlins, (423) 576-4507 P. F. Tortorelli, (423) 574-5119 Oak Ridge National Laboratory Contact: I. G. Wright, (423) 574-4451 The purpose of this task is to evaluate the high- University of Tennessee Contact: Peter Liaw, temperature corrosion behavior of iron-aluminum alloys (423) 974-6356 as part of the effort to develop highly corrosion-resistant iron-aluminide alloys and coatings for fossil energy The objective of this research is to characterize the applications. A primary objective is to investigate the fatigue and fracture behavior of Cr2Nb-based alloys and resistance of the alloys to mixed-oxidant (oxygen- other intermetallic materials at ambient and elevated sulfur-chlorine-carbon) environments that arise in the temperatures in controlled environments. These studies combustion or gasification of coal. This includes the are expected to lead to mechanistic understanding of determination of the influence of sulfur and other the fatigue and fracture behavior of these alloys. reactive gaseous species on corrosion kinetics and Fatigue tests shall be conducted for the purpose of oxide microstructures and the effects of alloying evaluating crack initiation and fatigue life of additions and oxide dispersoids on sulfidation and Cr2Nb-based alloys as well as other intermetallic alloys, oxidation resistance. The fatigue properties shall be evaluated as functions of test environment, cyclic frequency and test temperature. Keywords: Corrosion, Aluminides, Mixed-Gas, Scales Additional tensile tests will be required to characterize the fracture behavior of these structural alloys. Mechanical tests shall be performed to determine the fatigue and fracture behavior of Cr2Nb-based alloys.

'PYF denotes that funding for this project, active in FY 1997, was provided from prior year allocations.

185 Office of Fossil Energy

432. INVESTIGATION OF MOISTURE-INDUCED initial effort will be devoted to in situ composite alloys EMBRITTLEMENT OF IRON ALUMINIDES based on the Cr-Cr 2Nb system. $9,000 DOE Contacts: F. M. Glaser, (301) 903-2784 and Keywords: Corrosion, Chromium-Niobium, Mixed-Gas, M. H. Rawlins, (423) 576-4507 Scales Oak Ridge National Laboratory Contact: I. G. Wright, (423) 574-4451 435. OXIDE DISPERSION STRENGTHENED (ODS) Rensselaer Polytechnic Institute Contact: IRON ALUMINIDES N. S. Stoloff, (518) 276-6371 $295,000 DOE Contacts: F. M. Glaser, (301) 903-2784 and The purpose of this work is to study hydrogen embrittle- M. H. Rawlins, (423) 576-4507 ment of iron aluminide alloys. Moisture in air can Oak Ridge National Laboratory Contact: significantly reduce the room-temperature tensile I. G. Wright, (423) 574-4451 ductility of Fe3AI-based alloys by combining with the aluminum in the alloys to form atomic hydrogen. The The purpose of this task is to develop fabrication proce- atomic hydrogen diffuses rapidly into the material dures for making oxide dispersion-strengthened (ODS) causing embrittlement. Experiments are being iron-aluminum alloys based on Fe3AI. The suitability of conducted on selected Fe3AI alloys that will lead to an the procedures is measured in terms of the high- understanding of the phenomenon. The work focuses on emperature oxidation and sulfidation resistance and the effects of moisture on relevant mechanical creep strength of the ODS alloys compared with Fe3AI properties such as fatigue and tensile strengths, and alloys fabricated by conventional ingot and powder correlates important microstructural variables such as processes. degree of order, grain size, and phases present with the alloy's susceptibility to embrittlement. Keywords: Aluminides

Keywords: Aluminides, Embrittlement, Moisture 436. MATERIALS SUPPORT FOR HITAF $0 - PYF1 433. REDUCTION OF DEFECT CONTENT IN ODS DOE Contacts: F. M. Glaser, (301) 903-2784 and ALLOYS M. H. Rawlins, (423) 576-4507 $30,000 Oak Ridge National Laboratory Contact: DOE Contacts: F. M. Glaser, (301) 903-2784 and K. Breder, (423) 574-5089 M. H. Rawlins, (423) 576-4507 Oak Ridge National Laboratory Contact: This task involves the measurement of selected I. G. Wright, (423) 574-4451 mechanical and physical properties of structural The University of Liverpool Contact: A. R. Jones ceramics which are proposed for use in the construction of the High Temperature Advanced Furnace (HITAF) air The purpose of this work is to assess the sources of heater design being developed under the Combustion defects in oxide-dispersion-strengthened [ODS] alloys. 2000 Program. The purpose of the research is to Experiments to confirm key features of defects in ODS evaluate candidate structural ceramics for this alloys shall be devised and performed, and recommen- application by studying the fast fracture and fatigue dations shall be made for the reduction of defects in. (both dynamic and interrupted static) properties at these alloys. temperatures from 1100 to 1400°C in air, their corrosion behavior, property uniformity of components and long Keywords: Aluminides, Defects term degradation of ceramic properties due to exposure in prototype HITAF systems. 434. CORROSION PROTECTION OF ULTRAHIGH TEMPERATURE INTERMETALLIC ALLOYS Keywords: Furnace, Materials, HITAF $130,000 DOE Contacts: F. M. Glaser, (301) 903-2784 and M. H. Rawlins, (423) 576-4507 Oak Ridge National Laboratory Contact: P. F. Tortorelli, (423) 574-5119

The objective of this task is to develop high-strength, corrosion-resistant intermetallic alloys for use as hot components in advanced fossil energy conversion and combustion systems. The successful development of these alloys is expected to improve the thermal efficiency of fossil energy conversion systems through increased operating temperatures and to increase the service life of hot components exposed to corrosive environments at elevated temperatures (1000°C). The PYF denotes that funding for this project, active in FY 1997, was provided from prior year allocations.

186 Office of Fossil Energy

437. SUPPORT SERVICES FOR CERAMIC correlations between NDE results and failure of FIBER-CERAMIC MATRIX COMPOSITES specimens. $30,000 DOE Contacts: F. M. Glaser, (301) 903-2784 and Keywords: Nondestructive Evaluation, Ceramics, Flaws, M. H. Rawlins, (423) 576-4507 Fracture Oak Ridge National Laboratory Contact: D. P. Stinton, (423) 574-4556 DEVICE OR COMPONENT FABRICATION, University of North Dakota Energy and BEHAVIOR OR TESTING Environmental Research Center Contact: J. P. Hurley, (701) 777-5159 439. MATERIALS AND COMPONENTS IN FOSSIL ENERGYAPPLICATIONS NEWSLETTER This task will review and, if appropriate, propose modifi- $50,0001 cations to plans, materials, and tests planned by DOE Contacts: F. M. Glaser, (301) 903-2784 and researchers on the AR&TD Materials Program in work M. H. Rawlins, (423) 576-4507 to test materials for coal-fueled energy systems. The Oak Ridge National Laboratory Contact: changes shall be suggested in order to make the I. G. Wright, (423) 574-4451 corrosion experiments more reflective of the actual conditions that will be encountered by the materials in The purpose of this task is to publish a bimonthly, joint the energy systems. UNDEERC shall accomplish this DOE-Electric Power Research Institute (EPRI) task by reviewing the major advanced energy system newsletter to address current developments in materials projects being funded by the DOE, and by working with and components in fossil energy applications. Matching the company's technical monitor and staff to prepare a funding is provided by EPRI. summary of the expected corrosion problems. Both gasification and combustion systems will be included. Keywords: Materials, Components Ceramic materials in two subsystems will be the focus of this work: (1) hot gas cleanup systems and 440. DEVELOPMENT OF CERAMIC MEMBRANES (2) high-temperature heat exchangers. UNDEERC shall FOR GAS SEPARATION AND FUEL CELLS review and suggest improvements to materials testing $450,000 procedures that are used to determine material behavior DOE Contacts: F. M. Glaser, (301) 903-2784 and when used in hot-gas cleanup or heat exchanger M. H. Rawlins, (423) 576-4507 applications. A limited amount of computer modeling Oak Ridge National Laboratory Contact: and laboratory experimentation shall be a part of this R. R. Judkins, (423) 574-4572 effort. East Tennessee Technology Park Contact: D. E. Fain, (423) 574-9932 Keywords: Composites, Ceramics, Fibers The purpose of this activity is to fabricate inorganic 438. DEVELOPMENT OF NONDESTRUCTIVE membranes for the separation of gases at high EVALUATION METHODS AND EFFECTS OF temperatures and/or in hostile environments, typically FLAWS ON THE FRACTURE BEHAVIOR OF encountered in fossil energy conversion processes such STRUCTURAL CERAMICS as coal gasification. This work is performed in $180,000 conjunction with a separate research activity that is DOE Contacts: F. M. Glaser, (301) 903-2784 and concerned with the development and testing of the M. H. Rawlins, (423) 576-4507 ceramic membranes. Oak Ridge National Laboratory Contact: D. P. Stinton, (423) 574-4556 Keywords: Ceramics, Membranes, Filters, Separation, Argonne National Laboratory Contacts: Fuel Cells W. A. Ellingson, (708) 252-5068 J. P. Singh, (708) 252-5123

The purpose of this project is to study and develop acoustic and radiographic techniques and possible novel techniques such as nuclear magnetic resonance, to characterize structural ceramics with regard to presence of porosity, cracking, inclusions, amount of free silicon, and mechanical properties, and to establish the type and character of flaws that can be found by nondestructive evaluation (NDE) techniques. Both fired and unfired specimens are being studied to establish

'Matching funding provided by EPRI.

187 Office of Fossil Energy

441. EXTRUSION PRESS EQUIPMENT static and cyclic multiaxial loading at elevated $75,000 temperatures for extended time periods. DOE Contacts: F. M. Glaser, (301) 903-2784 and M. H. Rawlins, (423) 576-4507 Keywords: Ceramics, Composites, Mechanical Oak Ridge National Laboratory Contact: Properties, Testing R. R. Judkins, (423) 574-4572 East Tennessee Technology Park Contact: 444. SOLID STATE ELECTROLYTE SYSTEMS D. E. Fain, (423) 574-9932 $553,000 DOE This task provides funds for the procurement of major DOE Contacts: F. M. Glaser, (301) 903-2784 and equipment items, necessary for AR&TD Materials M. H. Rawlins, (423) 576-4507 Program activities. Oak Ridge National Laboratory Contact: R. R. Judkins, (423) 5744572 Keywords: Equipment Pacific Northwest National Laboratory Contact: L. R. Pederson, (509) 375-2579 442. HIGH-TEMPERATURE HEAT EXCHANGER AND HOT-GAS FILTER DEVELOPMENT The purpose of this project is to develop functional $0 - PYF 1 ceramic materials that will ultimately lead to the DOE Contacts: F. M. Glaser, (301) 903-2784 and broader, cleaner, and more efficient utilization of fossil M. H. Rawlins, (423) 576-4507 fuels, particularly coal and natural gas. This project is Oak Ridge National Laboratory Contact: composed of three principal tasks: D. P. Stinton, (423) 574-4556 Pennsylvania State University Contact: 1. Stability of Solid Oxide Fuel Cell Materials - R. E. Tressler, (814) 865-7961 The purpose of this task is to evaluate the stabilities of materials and interfaces in This project addresses the development of ceramic heat SOFCs in order to identify features that exchanger materials with chromia surface treatments would limit system performance. for corrosion resistance. High chromia-content refractories have been demonstrated to be resistant to 2. Mixed Oxyven lon/Electron-Conductina corrosion by coal slags. This project will focus on Ceramics for Oxyven Separation - improving the corrosion resistance of ceramics by Compositions and physical forms are being incorporating chromia into the surface layers. This work developed that simultaneously conduct has two principal parts: (1) screening analysis of oxygen ions and electrons. Such mixed candidate ceramic hot-gas filter materials, and (2) conducting ceramics can function as highly internal pressure testing of ceramic tubes exposed to selective oxygen separation membranes, coal combustion environments. allowing high purity oxygen to be separated from air. Keywords: Ceramics, Corrosion, Filters 3. Proton-Conducting Solid Electrolytes - This 443. INVESTIGATION OF THE MECHANICAL task will develop perovskite compositions PROPERTIES AND PERFORMANCE OF and physical forms, which will be used as CERAMIC COMPOSITE COMPONENTS the electrolyte in small-scale solid oxide fuel $ 0 - PYF' cells operating at intermediate temperatures. DOE Contacts: F. M. Glaser, (301) 903-2784 and M. H. Rawlins, (423) 576-4507 Keywords: Fuel Cells, SOFC Oak Ridge National Laboratory Contact: D. P. Stinton, (423) 574-4556 445. OXIDE-DISPERSION-STRENGTHENED Fe3AI- Virginia Polytechnic Institute Contact: BASED ALLOY TUBES K. L. Reifsnider, (703) 231-5259 $33,000 DOE Contacts: F. M. Glaser, (301) 903-2784 and The purpose of this project is to develop a test system M. H. Rawlins, (423) 576-4507 and test methods to obtain information on the properties Oak Ridge National Laboratory Contact: and performance of ceramic composite materials. The I. G. Wright, (423) 574-4451 work involves a comprehensive mechanical University of California at San Diego Contact: characterization of composite engineering components B. K. Kad, (619) 534-7059 such as tubes, plates, shells, and beams subjected to The goal of the work is to explore experimental and computational means by which inherent material and processing-induced anisotropies of ODS Fe3AI-base alloys can be exploited to meet in-service mechanical and creep-life requirements of the power generation 'PYF denotes that funding for this project, active in industry. The research shall examine microscopic and FY 1997, was provided from prior year allocations.

188 Office of Fossil Energy microstructural issues with a view to addressing 448. IRON ALUMINIDE FILTERS FOR PFBCs optimum material design for macroscopic components $50,000 under well prescribed in-service loading criteria. The DOE Contacts: F. M. Glaser, (301) 903-2784 and economic incentive is the low cost of Fe3AI-based alloys M. H. Rawlins, (423) 576-4507 and its superior sulfidation resistance, in comparison to Oak Ridge National Laboratory Contact: the competing Fe-Cr-AI base alloys and the Ni-base P.F. Tortorelli, (423) 574-5119 superalloys currently in service. The goal of this project is to determine the suitability of Keywords: Aluminide, Tubes particular iron aluminides as materials of construction for hot-gas filters in advanced first- and 446. ODS Fe3AI TUBES FOR HIGH-TEMPERATURE second-generation PFBCs. HEAT EXCHANGERS $50,000 Keywords: Filters, Aluminides DOE Contacts: F. M. Glaser, (301) 903-2784 and M. H. Rawlins, (423) 576-4507 449. CERAMIC TUBESHEET DESIGN ANALYSIS Oak Ridge National Laboratory Contact: $0 - PYF' I. G. Wright, (423) 574-4451 DOE Contacts: F. M. Glaser, (301) 903-2784 and PM Hochtemperatur-Metall. GmbH Contact: M. H. Rawlins, (423) 576-4507 Dieter Sporer, 011-43-5672-70-2923 Oak Ridge National Laboratory Contact: R. W. Swindeman, (423) 574-5108 The goal of the work is to produce tubes of Fe3AI-0.5 wt. percent Y203 which have properties suitable for The purpose of this task is to perform thermal and application as heat transfer surfaces in very high- mechanical analyses of critical regions in a ceramic temperature heat exchangers. The alloy is produced by tubesheet support for barrier filters in a hot gas cleanup a powder metallurgical (mechanical alloying) process, vessel designed for use in gasifier, carbonizer, and the main purpose of which is to obtain a uniform pressurized fluidized bed combustion gas streams. distribution of sub-micron Y203 particles in the Fe3AI matrix. The required high-temperature creep strength is Keywords: Ceramics, Tubesheet derived largely by developing very large, elongated grains which are effectively pinned by the oxide 450. DENSE CERAMIC TUBE DEVELOPMENT dispersion. Development of the necessary grain $100,000 structure is dependent on the characteristics of the DOE Contacts: F. M. Glaser, (301) 903-2784 and mechanically-alloyed powder, and on thermo- M. H. Rawlins, (423) 576-4507 mechanical processing of the consolidated powder. Oak Ridge National Laboratory Contact: T. M. Besmann, (423) 574-6852 Keywords: Aluminide, Tubes, Heat Exchangers The goal of this project is to demonstrate that 447. IRON ALUMINIDE FILTERS FOR IGCCs composite materials of high interest to the fossil energy $0 - PYF' community can be fabricated by chemical vapor DOE Contacts: F. M. Glaser, (301) 903-2784 and infiltration (CVI). Earlier work demonstrated that M. H. Rawlins, (423) 576-4507 composites could be fabricated in simple geometries Oak Ridge National Laboratory Contact: (thick-walled plates). However, more complex P. F. Tortorelli, (423) 574-5119 geometries were identified as important in a recent Continuous Fiber Ceramic Composite (CFCC) Initiative The purpose of this project is to provide technical report. Potentials applications for CFCCs include air support to the Pall Corporation in its development of heaters or recuperators, heat exchangers, catathermal porous sintered iron-aluminide filters for hot-particle or porous combustors, components for filtration removal from product streams in coal gasification systems, gas turbine components (primarily systems. The ORNL role is to provide specialized combustors), and radiant burner tubes. Nearly all of expertise in the areas of corrosion analysis, micro- these applications require tubular composites; therefore, structural characterization, alloy selection, and the process will be developed for the fabrication of processing based on extensive experience with iron tubular shapes. aluminides and materials performance in fossil energy systems. ORNL's contribution via this project should aid Keywords: Ceramics, Tubesheet the success and timely completion of Pall's development and demonstration efforts.

Keywords: Filters, Aluminides

'PYF denotes that funding for this project, active in FY 1997, was provided from prior year allocations.

189 Office of Fossil Energy

INSTRUMENTATION AND FACILITIES

451. MANAGEMENT OF THE FOSSIL ENERGY AR&TD MATERIALS PROGRAM $406,000 DOE Contacts: F. M. Glaser, (301) 903-2784 and M. H. Rawlins, (423) 576-4507 Oak Ridge National Laboratory Contact: R. R. Judkins, (423) 574-4572 The overall objective of the Fossil Energy Advanced Research and Technology Development (AR&TD) Materials program is to conduct a fundamental, long-range research and development program that addresses, in a generic way, the materials needs of fossil energy systems and ensures the development of advanced materials and processing techniques. The purpose of this task is to manage the Fossil Energy AR&TD Materials program in accordance with procedures described in the Program Management Plan approved by DOE. This task is responsible for preparing the technical program implementation plan for DOE approval; submitting budget proposals for the program; recommending work to be accomplished by subcon- tractors, other national laboratories, and by Oak Ridge National Laboratory (ORNL); placing and managing subcontracts for fossil energy materials development at industrial research centers, universities, and other government laboratories; and for reporting the progress of the program. Keywords: Management, Materials Program

452. GENERAL TECHNOLOGY TRANSFER ACTIVITIES $35,000 DOE Contacts: F. M. Glaser, (301) 903-2784 and M. H. Rawlins, (423) 576-4507 Oak Ridge National Laboratory Contact: R. R. Judkins, (423) 574-4572 The task provides funds for the initiation of technology transfer activities to identify and develop relationships with industrial partners for the transfer of AR&TD Materials Program technologies to industry.

Keywords: Technology Transfer

453. GORDON RESEARCH CONFERENCE SUPPORT $5,000 DOE Contacts: F. M. Glaser, (301) 903-2784 and M. H. Rawlins, (423) 576-4507 Oak Ridge National Laboratory Contact: R. R. Judkins, (423) 5744572

The task provides funds for partial support of the annual Gordon Research Conference.

Keywords: Technology Transfer

190 Directory